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Technical Notes
LEWATIT® GF 202 product is a methanol regenerable, adsorber resin that provides
crude biodiesel purification, absorbing residual free glycerin and associated soaps, salts
and water to achieve ASTM or EN specifications for B-100.

Biodiesel Purification

LEWATIT® GF 202 product is an adsorber resin with an affinity for residual free glycerin in crude
biodiesel. LEWATIT® GF 202 resin has a free glycerin adsorptive capacity of 200 - 250 grams
free glycerin/liter of resin, and is used to purify the phase separated and demethylated crude
biodiesel following transesterification. LEWATIT® GF 202 resin adsorbs residual free glycerin
and associated water, soaps, salts, etc. from the crude biodiesel, following (acid) neutralization
of the transesterification catalyst, phase separation of the crude biodiesel from crude glycerin
and the “rag layer” of soaps, and demethylation. The LEWATIT® GF 202 product is regenerated
using methanol, which is recovered and recycled, and is a highly cost effective alternative to
traditional water wash of the biodiesel. Residual free glycerin in the biodiesel following
purification with LEWATIT® GF 202 resin is about 50 PPM. LEWATIT® GF 202 resin is
expected to function for about five years with recommended methanol regeneration, and unlike
other dry wash resin systems, LEWATIT® GF 202 resin based crude biodiesel purification
process technology requires low residual methanol levels in the feed to be purified. LEWATIT®
GF 202 resin has an affinity for methanol, which is used to regenerate the resin when fully
loaded with adsorbed glycerin. Unlike other dry wash resin systems, LEWATIT® GF 202 resin
will not contribute to the acid number of the purified biodiesel, and will not revert soaps back to
FFA’s.

Post Transesterification Crude Biodiesel Treatment

Following transesterification, the reactor effluent should be processed as follows:

• Add just enough acid to neutralize the transesterification catalyst (shaken with water, the
water phase pH should be between 10 and 11).

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• Partially demethylate the transesterification reactor effluent to about to 2% methanol
(leave sufficient methanol to permit flowability of the glycerin phase following phase
separation).

• Phase separate the lighter crude biodiesel phase from the heavier crude glycerin phase
and soaps rag layer.
• Fully demethylate the isolated crude biodiesel to about 0.1% methanol.
• Phase separate the crude biodiesel a second time to remove additional phase separated
glycerin/soaps.

The crude biodiesel following the second phase separation should meet the specifications listed
in Table 1.

Table 1*
Crude Biodiesel Specifications
LEWATIT® GF 202 Resin Purification Bed
Preferred Maximum
<1,000 5,000
Residual Methanol
PPM PPM
Residual Free <1,250 2,500
Glycerin PPM PPM
Residual Soap** <250 PPM 500 PPM
Residual Salts** <250 PPM 500 PPM
Residual Moisture <250 PPM 500 PPM

*These items are provided as a general information only. They are approximate values and are not
considered part of the product specifications.
**Residual soaps and salts not to exceed 20% of the residual glycerin concentration.
This demethylated and phase separated crude biodiesel is then purified using LEWATIT® GF 202
resin to meet ASTM or EN specifications for B-100.

LEWATIT® GF 202 Resin Crude Biodiesel Purification Process Operating Guidelines

Recommended LEWATIT® GF 202 resin crude biodiesel purification process operating


guidelines are as follows:
• Operating process temperature 40 oC.

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o Processing temperature of 40 oC recommended to keep crude biodiesel viscosity
low, minimize pressure drop across the resin bed, and prevent adsorbed glycerin
from gelling.
• Crude biodiesel downflow throughput flowrates.
o Maximum throughput flowrate – 2 BV’s/Hr., regardless of residual free glycerin
content. BV’s are resin bed volumes/hour, and the resin bed volume is the
volume of resin in the column.
o 400 PPM to 1,000 PPM free glycerin – 2 BV’s/Hr.
o >1,000 PPM to 1,500 PPM free glycerin – 1.3 BV’s/Hr.
o >1,500 PPM to 2,000 PPM free glycerin – 1.0 BV’s/Hr.
o >2,000 PPM to 2,500 PPM free glycerin – 0.8 BV’s/Hr.
• LEWATIT® GF 202 resin bed depth - 3 meters (9.9 Ft.).
• Vessel sidewall height - 3.7 meters (12 Ft.).
o Provides 20% free space above the resin bed for expansion.
• Two columns operating in series – lead/lag configuration.
o Expected residual free glycerin in the purified biodiesel from LEWATIT® GF 202
resin based processing is approximately 50 PPM.
o When the lead column experiences breakthrough of residual free glycerin, it is
exhausted. Switch the lag column to the lead column position and regenerate
the exhausted lead column with methanol.

LEWATIT® GF 202 Resin Methanol Regeneration Process Operating Guidelines

Recommended LEWATIT® GF 202 resin methanol regeneration process operating guidelines


are as follows:
• Methanol regeneration volume – 5 BV’s.
• Methanol downflow regeneration flowrate - 2 to 3 BV’s/Hr.
• Methanol is drained from vessel followed by displacement with dry nitrogen.
• Methanol is rinsed from the resin with crude biodiesel at 2 to 4 BV’s/Hr. downflow for the
first 20-30 BV’s.

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• First 8 BV’s of crude biodiesel following methanol regeneration is recycled for methanol
strip, or prorationed back into crude feedstocks being fed to the transesterification
reactor.
• Next 13 to 20 BV’s methanol-rich biodiesel is diverted to storage for dilution, or
processed through the lag column.
• Methanol regeneration alternates between two columns operating in series.

Elution profile of LEWATIT® GF 202 Resin after Methanol Regeneration 
1,2
MeOH Strip or
Proration Recycle to Biodiesel to storage for blending, or to a
MeOH concentration in BD effluent (%)

1 Transesterification. second column of LEWATIT® GF 202


resin.

Throughput at 2 BV’s/Hr. downflow.


0,8

Throughput at 4 BV’s/Hr. downflow can be carried


0,6 out with freshly regenerated LEWATIT® GF 202
resin for the first 20-30 BV’s, diluting the MeOH
more quickly down to the specification value.

0,4 MeOH specification level.

0,2

0
0 5 10 15 20 25
Bed volumes biodiesel
*These items are provided as general information only. They are approximate values and are not
considered part of the product specifications.

LEWATIT® GF 202 Resin Bed Size Estimation Procedure for Crude Biodiesel Purification

1. Calculate the nominal free glycerin loading to the LEWATIT® GF 202 resin bed based on
the incoming residual free glycerin PPM, effluent residual free glycerin, and the nominal
flow rate of demethylated crude biodiesel expected.

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a. PPM free glycerin adsorbed on LEWATIT® GF 202 resin = incoming residual free
glycerin PPM – (minus) effluent residual free glycerin PPM. Nominal effluent
residual free glycerin is 50 PPM.
b. Grams/liter free glycerin adsorbed from incoming crude biodiesel = PPM free
glycerin adsorbed (from 1.a. above) x 1 gram/liter/1,000 PPM.
c. Grams/hour free glycerin adsorbed = grams/liter free glycerin adsorbed from
crude biodiesel (from 1.b. above) x throughput of incoming crude biodiesel in
liters/hour.
i. Liters/Hr. incoming crude biodiesel throughput = Gal./Hr. incoming crude
biodiesel x 3.785 Liters/Gal.
ii. Liters/Hr. incoming crude biodiesel throughput = Lbs./Hr. incoming crude
biodiesel throughput x 1 Gal./7.4 Lbs. crude biodiesel x 3.785 Liters/Gal.
2. Calculate the volume of LEWATIT® GF 202 resin required.
a. Select a desired methanol regeneration cycle time in hours. Our recommended
nominal regeneration cycle time is 128 hours.
b. LEWATIT® GF 202 resin free glycerin adsorptive capacity is 200 to 250 grams
free glycerin / liter LEWATIT® GF 202 resin.
c. Grams free glycerin adsorbed /methanol regeneration cycle = Grams/hour free
glycerin adsorbed (from 1.c. above) x desired methanol regeneration cycle time
in hours (from 2.a. above).
d. Liters LEWATIT® GF 202 resin required per column operating in a lead/lag
configuration = Grams free glycerin adsorbed/methanol regeneration cycle (from
2.c. above) / 200 grams free glycerin /liter LEWATIT® GF 202 resin.
e. Liters LEWATIT® GF 202 resin required for two columns in a lead/lag
configuration = 2 x Liters LEWATIT® GF 202 resin required per column in a
lead/lag configuration (from 2.d. above)
f. LEWATIT® GF 202 resin is packaged in 1,000-liter super sacks.
3. Calculation of LEWATIT® GF 202 resin column dimensions.
a. Column surface area (Sq. Meters) = Liters LEWATIT® GF 202 resin required per
column (from 2.d. above) x 1cubic meter/1,000 liters / 3 meters resin bed depth.
b. Column radius (meters) = square root of column resin bed surface area /
3.14159.
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c. Column diameter (meters) = 2 x column radius.
d. Column diameter (inches) = Column diameter (meters) x 39.37 inches/meter.
e. Adjust column diameter (inches) to closest standard size for top and bottom
heads. 
 

LEWATIT® GF 202 Resin Performance Example

The following LEWATIT® GF 202 resin crude biodiesel purification performance example is
based on a demethylated and phase separated crude biodiesel with a nominal quality of 1,250
PPM residual free glycerin maximum, 1,000 PPM residual methanol maximum, 250 PPM soaps
maximum, 250 PPM salts maximum, and 500 PPM residual moisture maximum, at nominal flow
rates of 500 Gal./Hr., 1,000 Gal./Hr., and 1,500 Gal./Hr., at 128 hours between methanol
regenerations. The demethylated and phase separated crude biodiesel is passed downflow
through LEWATIT® GF 202 resin (3 meters bed depth, 1.3 BV’s/Hr. and 40 0C).

Table 2*
LEWATIT® GF 202 Resin Crude Biodiesel Purification Performance Example
At 1,250 PPM Residual Free Glycerin, 1,000 PPM Residual Methanol,
250 PPM Soaps, 250 PPM Salts, and 500 PPM Residual Moisture

500 Gal./Hr. 1,000 Gal./Hr. 1,500 Gal./Hr.


LEWATIT® GF 202 resin requirements - 1,500 liters 3,000 liters 4,500 liters
liters/column
LEWATIT® GF 202 resin requirements - 3,000 liters 6,000 liters 9,000 liters
Total liters for two columns
LEWATIT® GF 202 resin bed depth 3 meters 3 meters 3 meters
Process throughput flow rate 1.3 BV’s/Hr. 1.3 BV’s/Hr. 1.3 BV’s/Hr.
Process operating temperature 40 0C 40 0C 40 0C
Nominal column diameter 2.5 Ft. 3.5 Ft. 4.5 Ft.
Nominal column sidewall height 12 Ft. 12 Ft. 12 Ft.
Nominal free glycerin in column effluent ≈ 50 PPM ≈ 50 PPM ≈ 50 PPM

*These items are provided as general information only. They are approximate values and are not
considered part of the product specifications.

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Table 3*
LEWATIT® GF 202 Resin Crude Biodiesel Purification Recommended Operating
Parameters

Recommended operating temperature 40 0C


LEWATIT® GF 202 resin bed depth 3 meters minimum
400 PPM to 1,000-PPM free glycerin, 2 BV’s/Hr.
Recommended purification bed >1,000 PPM to 1,500-PPM free glycerin, 1.3 BV’s/Hr.
throughput flow rate >1,500 PPM to 2,000 PPM free glycerin, 1 BV’s/Hr.
>2,000 PPM to 2,500 PPM free glycerin, 0.8 BV’s/Hr.
Free Space above resin bed 20% of resin bed depth

*These items are provided as general information only. They are approximate values and are not
considered part of the product specifications.

LEWATIT® GF 202 Resin Installation and Start-up Procedure

The following procedure is offered as a guide for installation and start-up of new or
replacement LEWATIT® GF 202 resin in a biodiesel polishing system. All precautions
required to safeguard personnel and/or the system should be taken prior to: inspection,
rinsing, performance of any required repairs or modifications, resin loading or process start-
up.

LEWATIT® GF 202 should be stored above 33oF, the operations described in this guide
must be carried out above freezing.

Vessel Inspection

1. Prior to removing the old resin from an existing system, record the height of the resin
bed in the vessel. This can be useful in determining the amount of replacement resin
required or diagnosing problems/issues with the existing bed by comparison with the
expected volume.
2. Completely remove old resin and any foreign material from the vessel and rinse the
vessel with approximately 5 BV of deionized water. Make sure to sweep away any
material clinging to walls, distributors and screens.

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3. Inspect headers, laterals, strainers and any other in-vessel equipment. Ensure they are
not loose, damaged, plugged or missing. Clean, tighten or repair as needed.

If possible, separately flow water through the system inlets and outlets at their respective
service flow rates and check flow patterns to ensure uniform flow distribution. Methanol and
feedstock pumps must be locked off. Vessel must be properly evacuated prior to any vessel
entry. Additional rinsing may be required if contaminants accumulate in the vessel during this
check.

Resin Loading

1. Record the volume and lot number of the resin to be used along with the vessel
identification for future reference.
2. Fill the vessel with sufficient demineralized water (approximately 1/3 the straight side
wall volume) to prevent resin breakage or internal distributor damage during loading.
3. Slowly load the specified volume of resin into the unit, taking care to remove the resin
from the packaging, making sure the water level is always above the top of the resin
bed.
4. Once the bed is loaded, make sure the water level is above the top of the bed and allow
the bed to soak for 2 to 4 hours.
5. Backwash, rinse up-flow, the resin with demineralized water at approximately 0.5 to 1
gpm/ft2 of bed area at water temperatures of 50 oF to 80 oF until the discharge from the
top of the vessel is clear and free of color (If backwash is not available due to piping
arrangements, a down flow rinse at the same flow rates and conditions will be sufficient).
Start the flow rate at 0.1 gpm/ft2 and slowly increase to establish a backwash flow rate
of 0.5 to 1 gpm/ft2. The backwash rate will vary depending on water temperature. Use
lower flow rates, 0.25 to 0.75 gpm/ft2 with colder water. Carefully monitor the backwash
effluent to ensure no loss of resin occurs. It is preferable to backwash through an open
man-way or through an open inlet distributor to allow the removal of any fine
contaminants. Check the backwash effluent frequently to ensure good resin is not being
backwashed from the vessel.

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6. Once the backwash is clear and free of color (this should take 5 to 10 bed volumes),
drain the water from the vessel. If possible, inspect the top of the resin bed to ensure
the resin surface is flat and at the correct level. Hills and valleys at the top of the bed
after backwash typically indicate uneven inlet flow distribution.
7. Residual water contained in the resin bed void volume can be removed by using
nitrogen or filtered dry compressed air flow through the vessel until the gas flow is
relatively free of water. Compressor oil contaminated air will foul the resin and can result
in poor performance.

Methanol Drying

1. Fill the vessel with dry methanol from the top of the vessel to the vessel top discharge
port and allow the resin to soak for 2 to 4 hours.
2. Rinse the resin with 4 additional bed volumes of dry methanol at 1.7 BV/hr. downflow
through the resin bed to complete resin methanol drying. This rinse step is required to
completely remove water from the resin bed prior to operation.

3. Drain the methanol from the vessel. Residual methanol contained in the resin bed void
volume can be removed by using nitrogen or filtered dry compressed air flow through the
vessel until the gas flow is relatively free of methanol. Compressor oil contaminated air
will foul the resin and can result in poor performance.

4. The methanol used during this dewatering step can be recovered and reused in the
process after drying.

Biodiesel Polishing System Start-up

1. Fill the vessel from the top with Biodiesel to be treated. Vent the vessel as it is filled.
Begin flowing biodiesel at design flow rate and temperature.

2. Sequester the first 3 – 5 bed volumes of biodiesel passed through the system and check
for methanol content. Blend as needed into the ongoing biodiesel stream.

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LEWATIT® GF 202 Resin Shut In Procedure

LEWATIT ® GF 202 Resin must not be left with biodiesel standing in the resin bed for a period
of time without flow through the resin bed.

If the LEWATIT ® GF 202 resin bed is to be placed in an idle or shut down mode, proper
procedures must be followed to prevent fouling of the resin bed and prevent potential oxidative
degradation of the contained biodiesel.
• Drain the biodiesel from the LEWATIT® GF 202 resin bed.
• Regenerate the resin bed using 5 BV’s of Methanol as recommended previously in these
Technical Notes.
• Use one of the following options to store the resin bed for future restart.
• Drain the Methanol from the resin bed, flush the resin bed with dry Nitrogen to drive out
residual Methanol, and seal off the resin bed under a dry Nitrogen blanket to prevent air
entering.
• Alternatively, leave the resin bed filled with Methanol, blanket the resin bed with dry
Nitrogen, and seal off the resin bed under a dry Nitrogen blanket to prevent air entering.

If the LEWATIT® GF 202 resin bed is to be taken off-line for a period not to exceed
approximately 16 hours, recirculate purified bidiesel through the resin bed at the normal
throughput rate in BV’s/Hr. and at the normal process temperature of 40 0C (104 0F). DO NOT
ALLOW AIR TO ENTER THE RESIN BED WHILE RECIRCULATING BIODIESEL. When the
resin bed is to be returned to regular service, switch back to feeding crude biodiesel.

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Additional Information and Regulations


Safety precautions
Strong oxidants, e.g. nitric acid, can cause violent reactions when in contact with ion exchange resins.

Toxicity
The material safety data sheet must be observed. The MSDS contains additional data on product
description, transport, storage, handling, safety and ecology.

Storage
It is recommended to store ion exchange resins at temperatures above the freezing point of water. Ion
exchange resins should not be stored in direct sunlight. If the resin should become frozen, the resin
should be left to thaw out at ambient temperature before handling. No attempt should be made to
accelerate the thawing process.

Disposal
The MSDS contains additional data on product safety and disposal.

MSDS
Material Safety Data Sheets are available for all Lanxess products. It is recommended that copies of the
MSDS be obtained by calling 1-800-678-0020 or 1-800-526-9377.

Health and Safety Information: Appropriate literature has been assembled which provides information concerning
the health and safety precautions that must be observed when handling the LANXESS products mentioned in this
publication. For materials mentioned which are not LANXESS products, appropriate industrial hygiene and other
safety precautions recommended by their manufacturers should be followed. Before working with any of these
products, you must read and become familiar with the available information on their hazards, proper use, and
handling. This cannot be overemphasized. Information is available in several forms, e.g., material safety data sheets
and product labels. Consult your LANXESS Corporation representative or contact the Product Safety and Regulatory
Affairs Department at LANXESS.

The manner in which you use and the purpose to which you put and utilize our products, technical assistance and information (whether
verbal, written or by way of production evaluations), including any suggested formulations and recommendations are beyond our control.
Therefore, it is imperative that you test our products, technical assistance and information to determine to your own satisfaction whether they
are suitable for your intended uses and application. This application-specific analysis must at least include testing to determine suitability
from a technical as well as health, safety, and environmental standpoint. Such testing has not necessarily been done by us. Unless we
otherwise agree in writing, all products are sold strictly pursuant to the terms of our standard conditions of sale. All information and technical
assistance is given without warranty or guarantee and is subject to change with notice. It is expressly understood and agreed that you
assume and hereby expressly release us from liability, in tort, contract or otherwise, incurred in connection with the use of our products,
technical assistance, and information. Any statement or recommendation not contained herein is unauthorized and shall not bind us.
Nothing herein shall be construed as a recommendation to use any product in conflict with patents covering any material or its use. No
license is implied or in fact granted under the claims of any patent.
®
LEWATIT is a registered trademark of LANXESS Deutschland GmbH.

LANXESS Sybron Chemicals Inc. LANXESS Corporation


200 Birmingham Road 111 RIDC Park West Drive
Birmingham, NJ 08011 Pittsburgh, PA 15275-1112
Phone: 1-800-678-0020 Phone: 1-800-526-9377
Fax: 1-609-894-8641 Fax: 1-412-809-1061

lewatit@lanxess.com www.US.lanxess.com
www.lewatit.com
www.sybronchemicals.com

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