CN202519181U - Device for continuously producing electronic grade propylene glycol methyl ether acetate - Google Patents
Device for continuously producing electronic grade propylene glycol methyl ether acetate Download PDFInfo
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- CN202519181U CN202519181U CN2012201004472U CN201220100447U CN202519181U CN 202519181 U CN202519181 U CN 202519181U CN 2012201004472 U CN2012201004472 U CN 2012201004472U CN 201220100447 U CN201220100447 U CN 201220100447U CN 202519181 U CN202519181 U CN 202519181U
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- China
- Prior art keywords
- propylene glycol
- monomethyl ether
- glycol monomethyl
- feed pump
- fresh feed
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The utility model discloses a device for continuously producing electronic grade propylene glycol methyl ether acetate. The device comprises a propylene glycol methyl ether charging pump (1), an acetic acid charging pump (2), a propylene glycol methyl ether preheater (3), an acetic acid preheater (4), a static mixer (5), a first fixed bed reactor (6), a second fixed bed reactor (7), a light removal tower charging pump (8), a light removal tower (9), a deionized tower charging pump (10) and a deionized tower (11). By adopting the device, the industrial production of electronic grade propylene glycol methyl ether acetate is realized, and the contents of metal ions such as Na, K, Ca, Mg, Pb, Zn, Fe and the like in the product are less than 10ppb, so that the requirement of electronic grade chemicals can be reached; the technology is simple in operation form, free from the processes of azeotropic dehydration and neutralization washing and high in production efficiency; the adopted composite solid acid catalyst is high in activity; and the device is good in mechanical strength, long in service life, energy-saving, environment-friendly and higher in economic benefit, and has good market prospect.
Description
Technical field
The utility model relates to a kind of preparation facilities of organic cpds, particularly relates to the device that the electronic grade propylene glycol monomethyl ether acetic ester is produced in a kind of serialization.
Background technology
The molecular formula of 1-Methoxy-2-propyl acetate is CH
3COOCH (CH
3) CH
2OCH
3It is the fine chemicals of one type of excellent property; It is the low toxicity advanced industrial solvent of excellent property; Because it has three the solvency power factor or groups that chemical functional is very strong---ehter bond, hydroxyl and ester group; Polarity and nonpolar material all there are very strong dissolving power, have the title of " omnipotent " solvent, be widely used in industrial circles such as coating, paint, printing ink, printing, dyestuff, leather, sensitive materials, electronic chemical product, senior clean-out system, synthetic brake fluid and additives for jet fuel as solvent or organic raw material.Therefore the toxicity of propylene glycol compounds will progressively replace the latter far below the glycol ether compounds.
The electronic grade propylene glycol monomethyl ether acetic ester has dissolving power very widely, its dissolution characteristics with respect to propylene glycol or ester class more near chlorinated solvents.In being applied to the photosensitive resin of semiconductor machining, electronic-grade PMA can be used to replace EEA, is mainly used in the processing of anode sensitive materials.The electronic grade propylene glycol monomethyl ether acetic ester also is used for liquid crystal display and photoresist material production process TFT-LCD photoresistance thinner, photo resistive removing liquor, stripper, industrial clean-out system, removing photoresistance damping fluid etc. and other special procure the chemical products of specification.Be widely used as the solvent of electronic material production usefulness simultaneously.
Generally adopt the homogeneous phase esterification reaction tech in the industry at present; Promptly adopting liquid acid such as sulfuric acid, hydrochloric acid, phosphoric acid, oxalic acid, Hydrocerol A and tosic acid is catalyzer (Liu Zhun etc.; Chinese patent CN1515537A; On July 28th, 2004), mainly there is long reaction time in this tradition homogeneous phase esterification reaction tech, by product is more, yield is not high, reaction product need add alkali neutralization, equipment corrosion is serious and problem such as product ion concentration severe overweight.In order to address the above problem, Wang Xi is used for the building-up reactions (Wang Xi, Liaoning teachers training school journal: natural science edition, 2000 the 2nd the 1st phases of volume) of 1-Methoxy-2-propyl acetate with heteropolyacid catalyst, and Gu Jingfang then adopts solid super-strong acid SO
4 2-/ TiO
2Catalyzer (Gu Jingfang, East China University of Science, master thesis, 2005) as the catalysis synthesizing propylene glycol monomethyl ether acetate it is reported, more than two kinds of catalyzer all have advantages of high catalytic activity, but heteropolyacid, solid super-strong acid SO
4 2-/ TiO
2Catalyzer is prone to poison, loss of active component, thereby causes work-ing life shorter, so do not see the report of industrial applications so far.Qin Xudong etc. use the catalyzer (Qin Xudong etc. of large hole cation exchanger resin as the industriallization 1-Methoxy-2-propyl acetate; Chinese patent CN101337885A; But whether the 1-Methoxy-2-propyl acetate product that obtains is satisfied electronic-grade require not make reports on January 7th, 2009).It is the electronic grade propylene glycol monomethyl ether acetic ester industrialized preparing process (Zhang Yong etc. of catalyzer with the strong-acid cation-exchange resin that Zhang Yong etc. disclose a kind of; Chinese patent CN101993360A; On August 21st, 2009); But comprise the azeotropic dehydration process of adding the band aqua in the described technology, the introducing of band aqua not only is unfavorable for environment protection, also incites somebody to action the yield of reduction 1-Methoxy-2-propyl acetate to a certain degree.
Summary of the invention
Technical problem: the purpose of the utility model provides the device that the electronic grade propylene glycol monomethyl ether acetic ester is produced in a kind of serialization, overcomes long reaction time in traditional homogeneous phase esterification reaction tech, by product is more, yield is not high, reaction product need add the alkali neutralization, need to add band aqua azeotropic dehydration, equipment corrosion is serious and problem such as product ion concentration severe overweight.
The device of electronic grade propylene glycol monomethyl ether acetic ester is produced in the utility model serialization, and it comprises propylene glycol monomethyl ether fresh feed pump, acetic acid fresh feed pump, propylene glycol monomethyl ether preheater, acetic acid preheater, static mixer, first fixed-bed reactor, second fixed bed reaction, lightness-removing column fresh feed pump, lightness-removing column, the sub-tower fresh feed pump of disengaging and breaks away from sub-tower;
Said propylene glycol monomethyl ether fresh feed pump, the parallel connection of acetic acid fresh feed pump are provided with; Said propylene glycol monomethyl ether fresh feed pump outlet links to each other with the import of propylene glycol monomethyl ether preheater; Said acetic acid charging pump outlet links to each other with the import of acetic acid preheater; The outlet of said propylene glycol monomethyl ether preheater and acetic acid preheater links to each other with the static mixer import respectively, said static mixer, first fixed-bed reactor, second fixed bed reaction, lightness-removing column fresh feed pump, lightness-removing column, the sub-tower fresh feed pump of disengaging and break away from the setting of connecting successively of sub-tower.
Said static mixer is a corrugated plate type, or the simple helix type, or double helical form, or horizontal stripe type static mixer.
Said static mixer coats thermal insulation layer outward.
Compared with prior art, the beneficial effect of the utility model:
The device of electronic grade propylene glycol monomethyl ether acetic ester is produced in the serialization of the utility model; Through the new type of continuous metallization processes; Realize the suitability for industrialized production of electronic grade propylene glycol monomethyl ether acetic ester; Metals ion in the product such as sodium, potassium, calcium, magnesium, lead, zinc, iron equal size reach requirement of electronic grade chemicals all less than 10ppb; The operation format of this technology is simple, no azeotropic dehydration and in and water washing process, production efficiency is high, used composite solid-acid catalyst active high, physical strength is good, the life-span is long, energy-conserving and environment-protective, economic benefit is higher, has good market outlook.
Description of drawings
Fig. 1 produces the device synoptic diagram of electronic grade propylene glycol monomethyl ether acetic ester for the utility model serialization.
In Fig. 1,1 is the propylene glycol monomethyl ether fresh feed pump, and 2 is the acetic acid fresh feed pump; 3 is the propylene glycol monomethyl ether preheater, and 4 is the acetic acid preheater, and 5 is static mixer; 6 is first fixed-bed reactor, and 7 is second fixed bed reaction, and 8 is the lightness-removing column fresh feed pump; 9 is lightness-removing column, and 10 for breaking away from sub-tower fresh feed pump, and 11 for breaking away from sub-tower.
Embodiment
Referring to Fig. 1; The device of electronic grade propylene glycol monomethyl ether acetic ester is produced in the utility model serialization, it mainly by propylene glycol monomethyl ether fresh feed pump 1, acetic acid fresh feed pump 2, propylene glycol monomethyl ether preheater 3, acetic acid preheater 4, static mixer 5, first fixed-bed reactor 6, second fixed bed reaction 7, lightness-removing column fresh feed pump 8, lightness-removing column 9, break away from sub-tower fresh feed pump 10 and break away from sub-tower 11 and form;
Said propylene glycol monomethyl ether fresh feed pump 1,2 parallel connections of acetic acid fresh feed pump are provided with; Said propylene glycol monomethyl ether fresh feed pump 1 outlet links to each other with 3 imports of propylene glycol monomethyl ether preheater; The outlet of said acetic acid fresh feed pump 2 links to each other with 4 imports of acetic acid preheater; The outlet of said propylene glycol monomethyl ether preheater 3 and acetic acid preheater 4 links to each other with static mixer 5 imports respectively, said static mixer 5, first fixed-bed reactor 6, second fixed bed reaction 7, lightness-removing column fresh feed pump 8, lightness-removing column 9, breaks away from sub-tower fresh feed pump 10 and breaks away from the setting of connecting successively of sub-tower 11.
Said static mixer 5 is a corrugated plate type, or the simple helix type, or double helical form, or horizontal stripe type static mixer, and static mixer coats thermal insulation layer outward.
All load composite solid-acid catalyst in said first fixed-bed reactor 6, second fixed bed reaction 7.
Adopt the step of the utility model device serialization production electronic grade propylene glycol monomethyl ether acetic ester following:
(1) a certain proportion of propylene glycol monomethyl ether and acetic acid pump into device by Ucar 35 fresh feed pump and acetic acid fresh feed pump respectively; Mix through static mixer after being preheating to assigned temperature respectively; First fixed bed that gets into the filling composite solid-acid catalyst carries out esterification, and reaction pressure is that normal pressure, temperature of reaction are 65～85 ℃;
The ratio of said propylene glycol monomethyl ether and acetic acid is the mol ratio 1:1～1:1.5 of propylene glycol monomethyl ether and acetic acid;
Said propylene glycol monomethyl ether is identical with acetic acid preheating assigned temperature, is 65～85 ℃;
Said composite solid-acid catalyst is a kind of loading type PS strong-acid cation-exchange resin, and this catalyzer is obtained on the PS strong-acid cation-exchange resin by active constituent loading;
Said active ingredient is a kind of in nickelous nitrate, aluminum nitrate, nitric acid tin and the zinc nitrate;
Each feed molar proportioning of said PS strong-acid cation-exchange resin is following, monomer styrene: linking agent Vinylstyrene: initiator Sodium Persulfate=85～94:5～15:1～3.
Esterification takes place rapidly in propylene glycol monomethyl ether and acetic acid under the effect of composite solid-acid catalyst; Because reaction reactant concn in early stage is higher and composite solid-acid catalyst is active higher; It is 70 ℃～80 ℃ that the service temperature in this stage maintains lower 65 ℃～85 ℃, preferred temperature, can make the esterification transformation efficiency reach 70%～85%;
Second fixed bed that (2) first fixed bed esterification products get into the filling composite solid-acid catalyst carries out esterification, and reaction pressure is that normal pressure, temperature of reaction are that 85～105 ℃, reaction velocity are 2～20 h
-1Above-mentioned first fixed bed directly links to each other with placed in-line form with second fixed bed, but two Solid Bed service temperatures are different.
Propylene glycol monomethyl ether and acetic acid continue to take place esterification under the effect of composite solid-acid catalyst; Because reaction late phase reaction substrate concentration is relatively low, thus need higher temperature to accelerate speed of reaction, but this esterification is thermopositive reaction; The too high meeting of temperature makes the balance of esterification to reactant one side shifting; Be unfavorable for obtaining high transformation efficiency, comprehensive above-mentioned two factors, the service temperature of selecting second fixed bed is 85 ℃～105 ℃; Be preferably 90 ℃～100 ℃, the conversion rate of esterification that can make the second fixed bed esterification products is greater than 99.5%;
(3) second fixed bed esterification products entering lightness-removing column removes the water of esterification generation, excessive acetic acid and a small amount of unreacted propylene glycol monomethyl ether; The lightness-removing column atmospheric operation; Operating reflux ratio 0.5～2.0; Preferable range is 0.8～1.5, and lightness-removing column top discharge light constituent below 140 ℃ is water, propylene glycol monomethyl ether and acetic acid, and 140～150 ℃ of components in lightness-removing column bottom are thick 1-Methoxy-2-propyl acetate;
(4) thick 1-Methoxy-2-propyl acetate gets into the sub-tower of disengaging and removes ion; Electron gain grade propylene glycol monomethyl ether acetic ester, the operational condition that breaks away from sub-tower is: atmospheric operation, operating reflux ratio 3.0～5.0; Preferable range is 3.5～4.5; Break away from sub-top of tower temperature-stable at 147.0～147.2 ℃, break away from sub-top of tower discharging and be the electronic grade propylene glycol monomethyl ether acetic ester, break away from per 24～48 h discharging of sub-tower bottom debris once.
Above-mentioned four processes are that raw material constantly pumps into device, the serialization production process of the continuous discharger of electronic grade propylene glycol monomethyl ether acetic ester product, and operation is investigated through pilot plant, and the life-span of this composite solid-acid catalyst is more than 3 years.
Claims (3)
1. the device of electronic grade propylene glycol monomethyl ether acetic ester is produced in a serialization, it is characterized in that: it comprises propylene glycol monomethyl ether fresh feed pump (1), acetic acid fresh feed pump (2), propylene glycol monomethyl ether preheater (3), acetic acid preheater (4), static mixer (5), first fixed-bed reactor (6), second fixed bed reaction (7), lightness-removing column fresh feed pump (8), lightness-removing column (9), breaks away from sub-tower fresh feed pump (10) and disengaging sub-tower (11);
Said propylene glycol monomethyl ether fresh feed pump (1), acetic acid fresh feed pump (2) parallel connection are provided with; Said propylene glycol monomethyl ether fresh feed pump (1) outlet links to each other with propylene glycol monomethyl ether preheater (3) import; The outlet of said acetic acid fresh feed pump (2) links to each other with acetic acid preheater (4) import; The outlet of said propylene glycol monomethyl ether preheater (3) and acetic acid preheater (4) links to each other with static mixer (5) import respectively, said static mixer (5), first fixed-bed reactor (6), second fixed bed reaction (7), lightness-removing column fresh feed pump (8), lightness-removing column (9), breaks away from the setting of connecting successively of sub-tower fresh feed pump (10) and the sub-tower of disengaging (11).
2. the device of electronic grade propylene glycol monomethyl ether acetic ester is produced in serialization according to claim 1, and it is characterized in that: said static mixer (5) is a corrugated plate type, or the simple helix type, or double helical form, or horizontal stripe type static mixer.
3. the device of electronic grade propylene glycol monomethyl ether acetic ester is produced in serialization according to claim 1 and 2, it is characterized in that: the outer thermal insulation layer that coats of said static mixer (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012201004472U CN202519181U (en) | 2012-03-17 | 2012-03-17 | Device for continuously producing electronic grade propylene glycol methyl ether acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012201004472U CN202519181U (en) | 2012-03-17 | 2012-03-17 | Device for continuously producing electronic grade propylene glycol methyl ether acetate |
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| Publication Number | Publication Date |
|---|---|
| CN202519181U true CN202519181U (en) | 2012-11-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012201004472U Expired - Lifetime CN202519181U (en) | 2012-03-17 | 2012-03-17 | Device for continuously producing electronic grade propylene glycol methyl ether acetate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018192195A1 (en) * | 2017-04-20 | 2018-10-25 | 江苏华伦化工有限公司 | Method for preparing semiconductor-grade propylene glycol methyl ether acetate |
| CN109134174A (en) * | 2017-06-16 | 2019-01-04 | 天津中福泰克化工科技有限公司 | It is a kind of for toluene/aceticanhydride/2- oxa- -1,4- diethyl-butanediol separation method and equipment |
| CN112194580A (en) * | 2020-11-04 | 2021-01-08 | 中建安装集团有限公司 | Device and process for producing propylene glycol monomethyl ether acetate by reactive distillation coupled pervaporation |
| CN115282895A (en) * | 2022-07-12 | 2022-11-04 | 铜陵贝斯美科技有限公司 | Device and production process for preparing amyl acetate from amylene and acetic acid |
-
2012
- 2012-03-17 CN CN2012201004472U patent/CN202519181U/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018192195A1 (en) * | 2017-04-20 | 2018-10-25 | 江苏华伦化工有限公司 | Method for preparing semiconductor-grade propylene glycol methyl ether acetate |
| CN109134174A (en) * | 2017-06-16 | 2019-01-04 | 天津中福泰克化工科技有限公司 | It is a kind of for toluene/aceticanhydride/2- oxa- -1,4- diethyl-butanediol separation method and equipment |
| CN112194580A (en) * | 2020-11-04 | 2021-01-08 | 中建安装集团有限公司 | Device and process for producing propylene glycol monomethyl ether acetate by reactive distillation coupled pervaporation |
| CN115282895A (en) * | 2022-07-12 | 2022-11-04 | 铜陵贝斯美科技有限公司 | Device and production process for preparing amyl acetate from amylene and acetic acid |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: JIANGSU YIDA CHEMICAL CO., LTD. Free format text: FORMER NAME: YIDA CHEMICAL CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 214444 Jiangsu city of Wuxi province Jiangyin City Li Gang Zhen Xi Shi Qiao ball Village No. 1 Patentee after: Jiangsu Yida Chemical Co., Ltd. Address before: 214444 Jiangsu city of Wuxi province Jiangyin City Li Gang Zhen Xi Shi Qiao ball Village No. 1 Patentee before: Yida Chemical Co., Ltd. |
|
| CX01 | Expiry of patent term |
Granted publication date: 20121107 |
|
| CX01 | Expiry of patent term |