CN111574338A - Dealcoholization rectification purification system and method for propylene glycol methyl ether production - Google Patents

Dealcoholization rectification purification system and method for propylene glycol methyl ether production Download PDF

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Publication number
CN111574338A
CN111574338A CN202010570334.8A CN202010570334A CN111574338A CN 111574338 A CN111574338 A CN 111574338A CN 202010570334 A CN202010570334 A CN 202010570334A CN 111574338 A CN111574338 A CN 111574338A
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China
Prior art keywords
dealcoholization
methanol
pipeline
propylene glycol
methyl ether
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CN202010570334.8A
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Chinese (zh)
Inventor
郑铁江
孙百亚
顾银军
吴晓明
汤宏良
周国君
万鹏
孙晓虎
陶植
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Jiangsu Baichuan High Tech New Materials Co ltd
Nantong Baichuan New Material Co ltd
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Jiangsu Baichuan High Tech New Materials Co ltd
Nantong Baichuan New Material Co ltd
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Priority to CN202010570334.8A priority Critical patent/CN111574338A/en
Publication of CN111574338A publication Critical patent/CN111574338A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01Preparation of ethers
    • C07C41/34Separation; Purification; Stabilisation; Use of additives
    • C07C41/40Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
    • C07C41/42Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation

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  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to the field of fine chemicals production, and particularly discloses a dealcoholization rectification purification system and a dealcoholization rectification purification method for propylene glycol methyl ether production, wherein the system comprises a methanol falling-film evaporator, a separator, a dealcoholization concentration liquid tank, a dealcoholization concentration liquid pump, a methanol condensate intermediate tank and a methanol condenser.

Description

Dealcoholization rectification purification system and method for propylene glycol methyl ether production
Technical Field
The invention relates to the production of propylene glycol methyl ether in the field of fine chemical production, in particular to a dealcoholization rectification purification system and a dealcoholization rectification purification method for propylene glycol methyl ether production.
Background
Propylene glycol methyl ether belongs to a glycol ether solvent, and the toxicity of propylene glycol ether to human bodies belongs to low-toxicity ethers. Propylene glycol methyl ether has weak ether smell but no strong pungent smell, so that the application of the propylene glycol methyl ether is wider and safer. Because the molecular structure of the polyether has ether group and hydroxyl group, the polyether has excellent solubility, proper volatilization rate, reaction activity and other characteristics, and thus has wide application.
Propylene glycol methyl ether is mainly used as a solvent, a dispersant and a diluent, and also used as a fuel antifreeze agent, an extractant and the like; is an intermediate of the herbicide metolachlor; used as solvent, dispersant or diluent in the industries of paint, ink, printing and dyeing, pesticide, cellulose, acrylate and the like. It can also be used as fuel antifreeze agent, cleaning agent, extractant, nonferrous metal beneficiation agent, etc. Can also be used as organic synthesis raw materials; the solvent is mainly used as an excellent solvent of nitrocellulose, alkyd resin and cis-anhydride modified phenolic resin, and is used as an anti-freezing agent of jet fuel, an additive of brake fluid and the like; the composite material is mainly used as a solvent, a dispersant and a diluent, and also used as a fuel antifreeze agent, an extractant and the like.
Propylene glycol methyl ether is produced into products and byproducts by adopting propylene oxide and methanol under the action of a catalyst in the production process, excess methanol (the molar ratio of propylene oxide to methanol is 1:3) needs to be subjected to a dealcoholization and recycling process, and the methanol distillation efficiency is related to the feeding amount of a front-stage process and the production amount of a subsequent process; therefore, it is necessary to select a dealcoholization rectification mode, which can not only improve the methanol separation speed in the production process, but also reduce the loss of methanol materials and maximize the yield.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a dealcoholization rectification purification system for propylene glycol methyl ether production to solve the problems in the background art.
The technical problem solved by the invention is realized by adopting the following technical scheme: a dealcoholize rectification purification system of propylene glycol methyl ether production includes: comprises a methanol falling-film evaporator, a separator, a dealcoholization concentrated solution tank, a dealcoholization concentrated solution pump, a methanol condensate intermediate tank and a methanol condenser,
the top of the methanol falling film evaporator is provided with a feed inlet, the left side of the methanol falling film evaporator is sequentially provided with a steam inlet and a condensed water outlet from top to bottom, the lower part of the right side of the methanol falling film evaporator is provided with a heavy component discharge port, and the bottom of the methanol falling film evaporator is provided with a non-dealcoholized material discharge port; the feed inlet is connected with a propylene glycol methyl ether etherification crude product feed pump through a pipeline A; the non-dealcoholized material discharge hole is connected with the pipeline A through a pipeline B;
the top of the separator is provided with a gas phase outlet, the side part of the separator is provided with a heavy component feed inlet, the bottom of the separator is provided with a dealcoholized liquid outlet, and the heavy component feed inlet is connected with the heavy component discharge outlet through a pipeline C;
the top of the dealcoholization concentrated liquid tank is provided with a dealcoholization liquid inlet, the bottom of the dealcoholization concentrated liquid tank is provided with a concentrated dealcoholization liquid outlet, the dealcoholization liquid inlet is connected with the dealcoholization liquid outlet through a pipeline E, the concentrated dealcoholization liquid outlet is connected with the dealcoholization concentrated liquid pump, and the dealcoholization concentrated liquid pump conveys the dealcoholization liquid to a subsequent working section through a pipeline F;
the methanol condenser top is equipped with the evacuation mouth, and left side upper portion is equipped with gaseous state methyl alcohol import, and the right side from top to bottom is equipped with cooling water export and cooling water import in proper order, and the bottom is equipped with liquid methyl alcohol export, gaseous state methyl alcohol import pass through pipeline D with gas phase exit linkage, liquid methyl alcohol export pass through pipeline G with methyl alcohol condensate intermediate tank connects, the evacuation mouth passes through pipeline L and is connected with vacuum system.
Furthermore, the number of the dealcoholization concentrate pumps is two, and the two dealcoholization concentrate pumps are connected to the pipeline F in parallel and can be switched for use; the dealcoholization concentrated solution pump is provided with a steam pressure gauge PI and a flow controller FC.
Furthermore, the steam inlet is connected with a steam heating device, and the condensed water outlet is connected with a steam condensed water recovery device.
Furthermore, the cooling water outlet is connected with a circulating water return system, and the cooling water inlet is connected with a circulating water upper water system.
Further, the dealcoholization concentrated solution tank is provided with a steam pressure gauge PI and a liquid level sensor LI.
Further, the methanol condensate intermediate tank is provided with a liquid level sensor LI.
Further, the pipeline E is provided with a sampling port.
A dealcoholization rectification purification method for propylene glycol methyl ether production adopts a dealcoholization rectification purification system for propylene glycol methyl ether production, and comprises the following steps:
s1: slowly pumping the propylene glycol methyl ether etherification crude product material into a methanol falling film evaporator;
s2: liquid dealcoholized heavy components and gaseous partial methanol enter a separator through a pipeline C, and the propylene glycol methyl ether etherification crude product material without dealcoholization enters a pipeline A through a pipeline B and is continuously thrown into a methanol falling-film evaporator;
s3: in the separator, a gaseous part of methanol enters a methanol condenser through a pipeline D, a liquid dealcoholization heavy component enters a dealcoholization concentrated liquid tank through a pipeline E, and then enters a subsequent working section through a dealcoholization concentrated liquid pump and finally a pipeline F;
s4: in the methanol condenser, methanol is converted from a gas phase to a liquid phase, and liquid methanol enters a methanol condensate intermediate tank through a pipeline G to be collected;
s5: sampling and analyzing the sampling liquid at the sampling port, judging the rectification effect, and analyzing to obtain that the content of the methanol material in the material after the propylene glycol methyl ether etherification crude product is dealcoholized is less than or equal to 1 percent.
Further, the feeding quantity of the propylene glycol methyl ether etherification crude product material is controlled by adjusting the frequency conversion of a propylene glycol methyl ether etherification crude product feeding pump, so that the temperature and the liquid level in the methanol falling film evaporator and the separator are stable.
Further, the temperature of the methanol falling-film evaporator is 110-120 ℃, the temperature of the feed inlet is 80-90 ℃, and the temperature of the gaseous methanol inlet is 50-60 ℃.
The invention has the beneficial effects that:
in the dealcoholization and rectification production process of the propylene glycol methyl ether etherification crude product, methanol is directly removed through a methanol falling film evaporator, and the temperature and liquid level in the methanol falling film evaporator and a separator can be regulated to be stable by controlling the feeding amount, so that reflux equipment in the existing rectification process is reduced, and the reflux temperature control process is also reduced.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed for the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a process flow for dealcoholizing a crude propylene glycol methyl ether etherification product of the present invention;
in the figure: 1-methanol falling film evaporator, 2-separator, 3-dealcoholization concentrated liquid tank, 4-dealcoholization concentrated liquid pump, 5-methanol condensate intermediate tank, 6-methanol condenser, 7-sampling port, 801-feed inlet, 802-steam inlet, 803-condensed water outlet, 804-heavy component discharge port, 805-undecoholization material discharge port, 806-gas phase outlet, 807-heavy component feed inlet, 808-dealcoholization liquid outlet, 809-dealcoholization liquid inlet, 810-concentrated dealcoholization liquid outlet, 811-gaseous methanol inlet, 812-cooling water outlet, 813-cooling water inlet, 814-vacuum pumping port and 815-liquid methanol outlet.
Detailed Description
The following describes the specific embodiments of the present invention with reference to examples, so that the technical solutions and the advantages thereof are more clear and clear. The following described embodiments are exemplary and are intended to be illustrative of the invention, but are not to be construed as limiting the invention.
Example (b):
as shown in fig. 1, the invention specifically discloses a dealcoholization rectification purification system for propylene glycol methyl ether production, which comprises a methanol falling-film evaporator 1, a separator 2, a dealcoholization concentrate tank 3, a dealcoholization concentrate pump 4, a methanol condensate intermediate tank 5 and a methanol condenser 6, wherein the number of the dealcoholization concentrate pumps 4 is two, and the two dealcoholization concentrate pumps 4 are connected in parallel on a pipeline F and can be switched for use; the dealcoholization concentrated solution pump 4 is provided with a steam pressure gauge PI and a flow controller FC; the dealcoholization concentrated liquid tank 3 is provided with a steam pressure gauge PI and a liquid level sensor LI; the methanol condensate intermediate tank 5 is provided with a liquid level sensor LI;
the top of the methanol falling film evaporator 1 is provided with a feed inlet 801, the left side is sequentially provided with a steam inlet 802 and a condensed water outlet 803 from top to bottom, the lower part of the right side is provided with a heavy component discharge port 804, and the bottom is provided with a non-dealcoholized material discharge port 805; a feed inlet 801 is connected with a propylene glycol methyl ether etherification crude product feed pump through a pipeline A; the undethanol material discharge port 805 is connected with the pipeline A through a pipeline B; the steam inlet 802 is connected with a steam heating device, and the condensed water outlet 803 is connected with a steam condensed water recovery device;
the top of the separator 2 is provided with a gas phase outlet 806, the side part is provided with a heavy component feed inlet 807, the bottom is provided with a dealcoholization liquid outlet 808, and the heavy component feed inlet 807 is connected with a heavy component discharge outlet 804 through a pipeline C;
the top of the dealcoholization concentrated liquid tank 3 is provided with a dealcoholization liquid inlet 809, the bottom of the dealcoholization concentrated liquid tank is provided with a concentrated dealcoholization liquid outlet 810, the dealcoholization liquid inlet 809 is connected with the dealcoholization liquid outlet 808 through a pipeline E, and the pipeline E is provided with a sampling port 7; the concentrated dealcoholized liquid outlet 810 is connected with a dealcoholized concentrated liquid pump 4, and the dealcoholized concentrated liquid pump 4 conveys the dealcoholized liquid to a subsequent working section through a pipeline F;
the top of the methanol condenser 6 is provided with a vacuumizing port 814, the upper part of the left side is provided with a gaseous methanol inlet 811, the right side is sequentially provided with a cooling water outlet 812 and a cooling water inlet 813 from top to bottom, the bottom is provided with a liquid methanol outlet 815, the gaseous methanol inlet 811 is connected with the gas phase outlet 806 through a pipeline D, the cooling water outlet 812 is connected with a circulating water return system, and the cooling water inlet 813 is connected with a circulating water upper water system; the liquid methanol outlet 815 is connected to the methanol condensate intermediate tank 5 via a pipe G, and the vacuum port 814 is connected to a vacuum system via a pipe L.
The dealcoholization rectification purification system for propylene glycol methyl ether production is adopted for purification, and comprises the following steps:
s1: slowly pumping the propylene glycol methyl ether etherification crude product material into a methanol falling film evaporator 1;
s2: liquid dealcoholized heavy components and gaseous partial methanol enter a separator 2 through a pipeline C, and the propylene glycol methyl ether etherification crude product material without dealcoholization enters a pipeline A through a pipeline B and is continuously injected into a methanol falling-film evaporator 1;
s3: in the separator 2, a gaseous part of methanol enters a methanol condenser 6 through a pipeline D, a liquid dealcoholization heavy component enters a dealcoholization concentrated liquid tank 3 through a pipeline E, and then enters a subsequent working section through a dealcoholization concentrated liquid pump 4 and finally a pipeline F;
s4: in the methanol condenser 6, methanol is converted from a gas phase to a liquid phase, and liquid methanol enters a methanol condensate intermediate tank 5 through a pipeline G to be collected;
s5: sampling and analyzing the sampling liquid at the sampling port 7, judging the rectification effect, and analyzing to obtain the methanol material content of 0.83% in the material after the propylene glycol methyl ether etherification crude product is dealcoholized.
In the steps S1-S4, the feeding quantity of the propylene glycol methyl ether etherification crude product material is controlled by adjusting the frequency conversion of the propylene glycol methyl ether etherification crude product feeding pump, so that the temperature and the liquid level in the methanol falling-film evaporator 1 and the separator 2 are stable.
Wherein in the steps S1-S4, the temperature of the methanol falling-film evaporator 1 is 110-120 ℃, the temperature of the feed inlet 801 is 80-90 ℃, and the temperature of the gaseous methanol inlet 811 is 50-60 ℃. The invention has the beneficial effects that:
in the dealcoholization and rectification production process of the propylene glycol methyl ether etherification crude product, methanol is directly removed through a methanol falling film evaporator, and the temperature and liquid level in the methanol falling film evaporator and a separator can be regulated to be stable by controlling the feeding amount, so that reflux equipment in the existing rectification process is reduced, and the reflux temperature control process is also reduced.
The above disclosure is only one preferred embodiment of the present invention, and certainly should not be construed as limiting the scope of the invention, which is defined by the claims and their equivalents.

Claims (10)

1. The dealcoholization rectification purification system for propylene glycol methyl ether production is characterized in that: comprises a methanol falling-film evaporator (1), a separator (2), a dealcoholization concentrated liquid tank (3), a dealcoholization concentrated liquid pump (4), a methanol condensate intermediate tank (5) and a methanol condenser (6),
the top of the methanol falling film evaporator (1) is provided with a feed inlet (801), the left side of the methanol falling film evaporator is sequentially provided with a steam inlet (802) and a condensed water outlet (803) from top to bottom, the lower part of the right side of the methanol falling film evaporator is provided with a heavy component discharge hole (804), and the bottom of the methanol falling film evaporator is provided with a non-dealcoholized material discharge hole (805); the feed inlet (801) is connected with a propylene glycol methyl ether etherification crude product feed pump through a pipeline A; the undethanolated material discharge hole (805) is connected with the pipeline A through a pipeline B;
the top of the separator (2) is provided with a gas phase outlet (806), the side part of the separator is provided with a heavy component feed inlet (807), the bottom of the separator is provided with a dealcoholization liquid outlet (808), and the heavy component feed inlet (807) is connected with the heavy component discharge outlet (804) through a pipeline C;
the top of the dealcoholization concentrated liquid tank (3) is provided with a dealcoholization liquid inlet (809), the bottom of the dealcoholization concentrated liquid tank is provided with a concentrated dealcoholization liquid outlet (810), the dealcoholization liquid inlet (809) is connected with the dealcoholization liquid outlet (808) through a pipeline E, the concentrated dealcoholization liquid outlet (810) is connected with the dealcoholization concentrated liquid pump (4), and the dealcoholization concentrated liquid pump (4) conveys the dealcoholization liquid to a subsequent working section through a pipeline F;
methanol condenser (6) top is equipped with evacuation mouth (814), and left side upper portion is equipped with gaseous state methyl alcohol import (811), and the right side from top to bottom is equipped with cooling water outlet (812) and cooling water inlet (813) in proper order, and the bottom is equipped with liquid methyl alcohol export (815), gaseous state methyl alcohol import (811) pass through pipeline D with gaseous phase export (806) are connected, liquid methyl alcohol export (815) pass through pipeline G with groove (5) are connected in the middle of the methyl alcohol condensate, evacuation mouth (814) pass through pipeline L and vacuum system connection.
2. The dealcoholization rectification purification system for propylene glycol methyl ether production according to claim 1, wherein the number of the dealcoholization concentrate pumps (4) is two, and the two dealcoholization concentrate pumps (4) are connected in parallel to the pipeline F and can be switched for use; the dealcoholization concentrated solution pump (4) is provided with a steam pressure gauge PI and a flow controller FC.
3. The dealcoholization rectification purification system for producing propylene glycol methyl ether according to claim 1, wherein the steam inlet (802) is connected with a steam heating device, and the condensed water outlet (803) is connected with a steam condensed water recovery device.
4. The dealcoholization rectification purification system for the production of propylene glycol methyl ether according to claim 1, wherein the cooling water outlet (812) is connected with a circulating water return system, and the cooling water inlet (813) is connected with a circulating water upper water system.
5. The dealcoholization rectification purification system for propylene glycol methyl ether production according to claim 1, wherein the dealcoholization concentrate tank (3) is provided with a steam pressure gauge PI and a liquid level sensor LI.
6. The dealcoholization rectification purification system for the production of propylene glycol methyl ether according to claim 1, wherein the methanol condensate intermediate tank (5) is provided with a liquid level sensor LI.
7. The dealcoholization rectification purification system for the production of propylene glycol methyl ether according to claim 1, wherein the pipeline E is provided with a sampling port (7).
8. A dealcoholization rectification purification method for propylene glycol methyl ether production adopts the dealcoholization rectification purification system for propylene glycol methyl ether production of any one of claims 1 to 7 for purification, and is characterized in that: the purification method comprises the following steps:
s1: slowly pumping the propylene glycol methyl ether etherification crude product material into a methanol falling film evaporator (1);
s2: liquid dealcoholized heavy components and gaseous partial methanol enter a separator (2) through a pipeline C, and the undecoholized propylene glycol methyl ether etherification crude product material enters a pipeline A through a pipeline B and is continuously thrown into a methanol falling-film evaporator (1);
s3: in the separator (2), a gaseous part of methanol enters a methanol condenser (6) through a pipeline D, a liquid dealcoholization heavy component enters a dealcoholization concentrated liquid tank (3) through a pipeline E, then passes through a dealcoholization concentrated liquid pump (4), and finally enters a subsequent working section through a pipeline F;
s4: in the methanol condenser (6), methanol is converted from a gas phase to a liquid phase, and liquid methanol enters a methanol condensate intermediate tank (5) through a pipeline G to be collected;
s5: sampling and analyzing the sampling liquid of the sampling port (7), judging the rectification effect, and analyzing to obtain that the content of the methanol material in the material after the propylene glycol methyl ether etherification crude product is dealcoholized is less than or equal to 1 percent.
9. The method for dealcoholizing, rectifying and purifying the propylene glycol methyl ether production according to claim 8, wherein the feeding amount of the propylene glycol methyl ether etherification crude product is controlled by adjusting the frequency conversion of a propylene glycol methyl ether etherification crude product feeding pump, so that the temperature and the liquid level in the methanol falling film evaporator (1) and the separator (2) are stable.
10. The method for the dealcoholization, rectification and purification of propylene glycol methyl ether production as recited in claim 9, wherein the temperature of the methanol falling-film evaporator (1) is 110-120 ℃, the temperature of the feed inlet (801) is 80-90 ℃, and the temperature of the gaseous methanol inlet (811) is 50-60 ℃.
CN202010570334.8A 2020-06-22 2020-06-22 Dealcoholization rectification purification system and method for propylene glycol methyl ether production Pending CN111574338A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115784851A (en) * 2022-10-28 2023-03-14 南通百川新材料有限公司 Novel propylene glycol methyl ether rectification production method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613259A (en) * 2008-06-27 2009-12-30 江苏瑞佳化学有限公司 The preparation method of electronic grade propylene glycol monomethyl ether

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN101613259A (en) * 2008-06-27 2009-12-30 江苏瑞佳化学有限公司 The preparation method of electronic grade propylene glycol monomethyl ether

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
房鼎业等: "《甲醇生产技术及进展》", vol. 1990, 31 October 1990, 华东化工学院出版社, pages: 319 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115784851A (en) * 2022-10-28 2023-03-14 南通百川新材料有限公司 Novel propylene glycol methyl ether rectification production method
CN115784851B (en) * 2022-10-28 2024-04-05 南通百川新材料有限公司 Propylene glycol methyl ether rectification production method

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