CN107459460A - A kind of process for purification of the tricaprylate of triethylene glycol two - Google Patents
A kind of process for purification of the tricaprylate of triethylene glycol two Download PDFInfo
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- CN107459460A CN107459460A CN201710927907.6A CN201710927907A CN107459460A CN 107459460 A CN107459460 A CN 107459460A CN 201710927907 A CN201710927907 A CN 201710927907A CN 107459460 A CN107459460 A CN 107459460A
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- triethylene glycol
- tricaprylate
- purification
- temperature
- reaction bulb
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of process for purification of the tricaprylate of triethylene glycol two, comprise the following steps：The first step, crude product is made as raw material using triethylene glycol and isooctyl acid；Second step, molecular distillation purification is carried out to crude product；3rd step, complete the preparation of the tricaprylate final products of triethylene glycol two.In traditional preparation method, the tricaprylate of triethylene glycol two easily produces a large amount of waste water by the conventional method for washing that neutralizes, pollute environment, steam distillation method temperature is too high to be prone to side reaction, influences properties of product, and with the method for purification of the present invention, product purity is high, colourity is good, without being decolourized, good product performance.
Description
Technical field
The present invention relates to a kind of preparation method of the tricaprylate of triethylene glycol two, more particularly to a kind of tricaprylate of triethylene glycol two
Process for purification.
Background technology
The tricaprylate of triethylene glycol two is solvent-borne type cold resistant plasticizer, has excellent low temperature properties, durability, oil resistivity, resistance to
Ultraviolet irradiates and antistatic behaviour, and has the characteristics that the low and certain lubricity of viscosity.Its molecular structure can make plastic product
With good colourity and the transparency.With resin similar in polarity make it good with resin intermiscibility, thus be widely used in PVB
The multiple fields such as safety diaphragm, synthetic rubber, vinylite, PVC, industrial coating coating, encapsulant.Production both at home and abroad at present
The production post-processing approach that enterprise uses is neutralized for traditional alkali cleaning, washed, dehydration, is produced a large amount of waste liquids, is caused environmental pollution,
And it is serious to equipment corrosion, potential safety hazard be present, product quality is relatively low.
The content of the invention
The present invention proposes a kind of process for purification of the tricaprylate of triethylene glycol two, solves domestic and international manufacturing enterprise at present and adopts
Production post-processing approach is that traditional alkali cleaning is neutralized, washes, is dehydrated, and produces a large amount of waste liquids, causes environmental pollution, and right
Equipment corrosion is serious, the problem of potential safety hazard, product quality is relatively low be present.
In order to solve the above-mentioned technical problem, the invention provides following technical scheme：
A kind of process for purification of the tricaprylate of triethylene glycol two of the present invention, comprises the following steps：
The first step, make crude product；Second step, carry out molecular distillation purification；3rd step, it is final to complete the tricaprylate of triethylene glycol two
The making of product.
As a preferred technical solution of the present invention, prepare equipment and material：Needed to use in manufacturing process to a system
Row equipment and various materials, before the experiment of the tricaprylate of triethylene glycol two make, equipment and material are first got out in advance；Device
Material includes Precision Electronics Balance, reaction bulb, nitrogen cylinder, agitator, heating water tank, temperature sensor, cold water storage cistern, vacuum distillation dress
Put, filter, molecular distillation apparatus, vacuum measurement instrument, collecting bottle and drying device；Material includes isooctyl acid, triethylene glycol, height
Imitate solid super acid catalyst and water entrainer.
As a preferred technical solution of the present invention, crude product is made：2.1-2.3 in molar ratio:1 by isooctyl acid, three
Glycol is added in reaction bulb, meanwhile, add the high-performance solid super acidic catalysts of 1-2 ‰, 1-2% adsorbents and 5-10% band water
Agent, then under conditions of logical nitrogen, stirred by agitator, and reaction bulb is heated by heating water tank, make to send out in reaction bulb
Raw esterification dehydration；Then the temperature gone out with temperature sensor measurement in heating water tank, and keep the temperature in heating water tank
For 200-240 DEG C, the reaction bulb after generation esterification dehydration is set to be incubated 5-10 hours at such a temperature, then again by cold water storage cistern
Interior cold water is added in heating water tank, reduces the temperature in heating water tank, so as to cool to reaction bulb, and keeps anti-
Environment temperature where answering bottle is 80-150 DEG C, and the mixing liquid in reaction bulb then is poured into vacuum distillation at such a temperature again
It is evaporated under reduced pressure in device, sloughing water entrainer by 0.5-2 hours obtains crude product.
As a preferred technical solution of the present invention, molecular distillation purification：The crude product that making obtains was first passed through
Filter filters, and the crude product after filtering then is carried out into secondary molecules distillation by molecular distillation apparatus again, and pass by temperature
It is 50-120 DEG C that sensor, which keeps coagulation temperature, then it is 50- to be measured by vacuum measurement instrument and keep vacuum pressure
1000Pa so that remaining water entrainer and part acid are deviate from；Then two stage treatment is carried out again, is maintained at two stage treatment temperature
90-180 DEG C, vacuum pressure is maintained at 1-300Pa, so as to deviate from excess acid, obtains product acid number and is less than 0.1mg KOH/g.
As a preferred technical solution of the present invention, the making of the tricaprylate final products of triethylene glycol two is completed：It will divide
Being filtered from product using filter, obtain product acid number less than 0.1, platinum cobalt color number is less than 30, then through drying device drying and dehydrating
Final products are obtained, purity is more than 99%.
The beneficial effect that is reached of the present invention is：In traditional preparation method, the tricaprylate of triethylene glycol two passes through in routine
A large amount of waste water are easily produced with method for washing, pollute environment, steam distillation method temperature is too high to be prone to side reaction, influences to produce
Moral character energy, and it is high with the molecular distillation Methods For Purification of the present invention, product purity, colourity is good, without being decolourized, properties of product
It is good.
Embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment
The present invention provides a kind of process for purification of the tricaprylate of triethylene glycol two, comprises the following steps：
The first step, make crude product；Second step, carry out molecular distillation purification；3rd step, it is final to complete the tricaprylate of triethylene glycol two
The making of product.
Prepare equipment and material：A series of equipment and various materials are needed to use in manufacturing process, are carrying out making three
Before the experiment of the tricaprylate of glycol two, equipment and material are first got out in advance；Equipment includes Precision Electronics Balance, reaction bulb, nitrogen
Bottle, agitator, heating water tank, temperature sensor, cold water storage cistern, vacuum distillation apparatus, filter, molecular distillation apparatus, vacuum
Measuring instrument, collecting bottle and drying device；Material includes isooctyl acid, triethylene glycol, high-performance solid super acidic catalyst and water entrainer.
Make crude product：2.1-2.3 in molar ratio:1 adds isooctyl acid, triethylene glycol in reaction bulb, meanwhile, add 1-
2 ‰ high-performance solid super acidic catalysts, 1-2% adsorbents and 5-10% water entrainers, then under conditions of logical nitrogen, pass through agitator
Stirring, and reaction bulb is heated by heating water tank, make esterification dehydration occurs in reaction bulb；Then surveyed with temperature sensor
The temperature in heating water tank is measured, and it is 200-240 DEG C to keep the temperature in heating water tank, after making generation esterification dehydration
Reaction bulb is incubated 5-10 hours at such a temperature, and then the cold water in cold water storage cistern is added in heating water tank again, makes heating water
Temperature in case reduces, and so as to cool to reaction bulb, and the environment temperature where keeping reaction bulb is 80-150 DEG C, then
The mixing liquid in reaction bulb is poured into vacuum distillation apparatus at such a temperature again and is evaporated under reduced pressure, by 0.5-2 hours
Slough water entrainer and obtain crude product.
Molecular distillation purifies：The crude product that making obtains is first passed through into filter filtering, then again by the thick production after filtering
Product carry out secondary molecules distillation by molecular distillation apparatus, and it is 50- to keep coagulation temperature by temperature sensor
120 DEG C, then it is 50-1000Pa to be measured by vacuum measurement instrument and keep vacuum so that the sour quilt of remaining water entrainer and part
Abjection；Then two stage treatment is carried out again, two stage treatment temperature is maintained at 90-180 DEG C, vacuum is maintained at 1-300Pa, so as to
Deviate from most of excess acid, obtain product acid number acid number and be less than 0.1 mg KOH/g.
Complete the making of the tricaprylate final products of triethylene glycol two：Filtered using filter, obtain product acid number less than 0.1
Mg KOH/g, platinum cobalt color number is less than 30, then obtains final products through drying device drying and dehydrating, and purity is more than 99%.
The process for purification of the tricaprylate of triethylene glycol two of the present invention, in traditional preparation method, the tricaprylate of triethylene glycol two
A large amount of waste water are easily produced by the conventional method for washing that neutralizes, pollute environment, steam distillation method temperature is too high to be prone to pair
Reaction, properties of product are influenceed, and it is high with the molecular distillation Methods For Purification of the present invention, product purity, and colourity is good, without being taken off
Color, good product performance.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in the present invention's
Within protection domain.
Claims (5)
1. a kind of process for purification of the tricaprylate of triethylene glycol two, it is characterised in that comprise the following steps：
The first step, make crude product；Second step, carry out molecular distillation purification；3rd step, it is final to complete the tricaprylate of triethylene glycol two
The preparation of product.
2. the process for purification of the tricaprylate of a kind of triethylene glycol two according to claim 1, it is characterised in that utilize different pungent
Acid, triethylene glycol, high-performance solid super acidic catalyst, adsorbent and water entrainer are that raw material carries out esterification and prepares thick ester, and
Separating-purifying is carried out with molecular distillation.
3. the process for purification of the tricaprylate of a kind of triethylene glycol two according to claim 2, it is characterised in that make thick production
Product：2.1-2.3 in molar ratio:1 adds isooctyl acid, triethylene glycol in reaction bulb, meanwhile, it is superpower to add the high-performance solids of 1-2 ‰
Acid catalyst, 1-2% adsorbents and 5-10% water entrainers, then under conditions of logical nitrogen, stirred by agitator, and by adding
Boiler heats to reaction bulb, makes esterification dehydration occurs in reaction bulb；Then heating water tank is gone out with temperature sensor measurement
Interior temperature, and it is 200-240 DEG C to keep the temperature in heating water tank, makes the reaction bulb after generation esterification dehydration in the temperature
Degree lower insulation 5-10 hours, then the cold water in cold water storage cistern is added in heating water tank again, drops the temperature in heating water tank
Low, so as to cooling to reaction bulb, and the environment temperature where keeping reaction bulb is 80-150 DEG C, then again at such a temperature
Mixing liquid in reaction bulb is poured into vacuum distillation apparatus and is evaporated under reduced pressure, sloughing water entrainer by 0.5-2 hours obtains
To crude product.
4. the process for purification of the tricaprylate of a kind of triethylene glycol two according to claim 3, it is characterised in that molecular distillation carries
It is pure：The crude product that making obtains is first passed through into filter filtering, the crude product after filtering is then passed through into molecular distillation apparatus again
Secondary molecules distillation is carried out, and it is 50-120 DEG C to keep coagulation temperature by temperature sensor, then pass through vacuum
It is 50-1000Pa that measuring instrument, which measures and keeps vacuum pressure, so that remaining water entrainer and part acid are deviate from；Then two are carried out again
Level processing, makes two stage treatment temperature be maintained at 90-180 DEG C, vacuum pressure is maintained at 1-300Pa, so as to deviate from most of excess
Acid, obtain product acid number and be less than 0.1 mg KOH/g.
5. the process for purification of the tricaprylate of a kind of triethylene glycol two according to claim 4, it is characterised in that complete triethylene glycol
The making of two tricaprylate final products：Filtered using filter, obtain product acid number and be less than 0.1 mg KOH/g, platinum cobalt color number
Final products are obtained less than 30, then through drying device drying and dehydrating, purity is more than 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710927907.6A CN107459460A (en) | 2017-10-09 | 2017-10-09 | A kind of process for purification of the tricaprylate of triethylene glycol two |
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| CN201710927907.6A CN107459460A (en) | 2017-10-09 | 2017-10-09 | A kind of process for purification of the tricaprylate of triethylene glycol two |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109486436A (en) * | 2018-10-15 | 2019-03-19 | 宏和电子材料科技股份有限公司 | Electronic-grade glass yarn bonding agent and preparation method thereof |
| CN110015957A (en) * | 2019-03-30 | 2019-07-16 | 镇江巨杰新材料技术研发中心(有限合伙) | A kind of synthetic method and application of polyethylene glycol 400 tricaprylate |
| CN111393294A (en) * | 2020-04-13 | 2020-07-10 | 盘锦洪鼎化工有限公司 | Method for refining triethylene glycol diisocaprylate rectifying still residual liquid |
| CN111499507A (en) * | 2020-05-25 | 2020-08-07 | 东营市金凤凰化工股份有限公司 | Production process of diethylene glycol monobutyl ether adipate |
| CN113754536A (en) * | 2021-09-08 | 2021-12-07 | 孟永财 | Preparation method of triethylene glycol di-n-caprylate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102030638A (en) * | 2010-11-18 | 2011-04-27 | 浙江皇马科技股份有限公司 | Preparation process of neopentyl polyacohol octocapric acid ester |
| CN104529760A (en) * | 2014-12-03 | 2015-04-22 | 营口天元化工研究所股份有限公司 | Preparation method of triethylene glycol di-2-ethylhexoate |
| CN106431905A (en) * | 2016-08-11 | 2017-02-22 | 无锡市伟峰化工有限公司 | Preparation method of environment-friendly plasticizer-triethylene glycol di-2-ethylhexoate |
-
2017
- 2017-10-09 CN CN201710927907.6A patent/CN107459460A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030638A (en) * | 2010-11-18 | 2011-04-27 | 浙江皇马科技股份有限公司 | Preparation process of neopentyl polyacohol octocapric acid ester |
| CN104529760A (en) * | 2014-12-03 | 2015-04-22 | 营口天元化工研究所股份有限公司 | Preparation method of triethylene glycol di-2-ethylhexoate |
| CN106431905A (en) * | 2016-08-11 | 2017-02-22 | 无锡市伟峰化工有限公司 | Preparation method of environment-friendly plasticizer-triethylene glycol di-2-ethylhexoate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109486436A (en) * | 2018-10-15 | 2019-03-19 | 宏和电子材料科技股份有限公司 | Electronic-grade glass yarn bonding agent and preparation method thereof |
| CN110015957A (en) * | 2019-03-30 | 2019-07-16 | 镇江巨杰新材料技术研发中心(有限合伙) | A kind of synthetic method and application of polyethylene glycol 400 tricaprylate |
| CN111393294A (en) * | 2020-04-13 | 2020-07-10 | 盘锦洪鼎化工有限公司 | Method for refining triethylene glycol diisocaprylate rectifying still residual liquid |
| CN111393294B (en) * | 2020-04-13 | 2022-09-02 | 盘锦洪鼎化工有限公司 | Method for refining triethylene glycol diisocaprylate rectifying still residual liquid |
| CN111499507A (en) * | 2020-05-25 | 2020-08-07 | 东营市金凤凰化工股份有限公司 | Production process of diethylene glycol monobutyl ether adipate |
| CN113754536A (en) * | 2021-09-08 | 2021-12-07 | 孟永财 | Preparation method of triethylene glycol di-n-caprylate |
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| SE01 | Entry into force of request for substantive examination | ||
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| CB02 | Change of applicant information |
Address after: 528300 2 Daliang Road, five Sha Road, Shunde District, Foshan, Guangdong. Applicant after: Guangdong Fu Yan Sheng Technology Co., Ltd. Address before: 528308 2 Daliang Road, five Sha Road, Shunde District, Foshan, Guangdong. Applicant before: Foshan Shunde Fuyansheng Lubricant Co., Ltd. |
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| CB02 | Change of applicant information | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171212 |
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| RJ01 | Rejection of invention patent application after publication |