CN109293505A - The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate - Google Patents

The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate Download PDF

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Publication number
CN109293505A
CN109293505A CN201811373365.3A CN201811373365A CN109293505A CN 109293505 A CN109293505 A CN 109293505A CN 201811373365 A CN201811373365 A CN 201811373365A CN 109293505 A CN109293505 A CN 109293505A
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CN
China
Prior art keywords
ethylene glycol
citrate
microwave heating
container
functional
Prior art date
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Withdrawn
Application number
CN201811373365.3A
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Chinese (zh)
Inventor
蒲鉴
蒲霏嫣
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Qianxi Guizhou Coal Chemical Investment Co Ltd
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Qianxi Guizhou Coal Chemical Investment Co Ltd
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Priority to CN201811373365.3A priority Critical patent/CN109293505A/en
Publication of CN109293505A publication Critical patent/CN109293505A/en
Withdrawn legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/52Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10General cosmetic use

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • Animal Behavior & Ethology (AREA)
  • Emergency Medicine (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Dermatology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses the techniques for utilizing microwave heating technique production ethylene glycol citrate to be used for cosmetics, comprising the following steps: S1: fresh lemon is taken then to utilize squeezer that lemon is squeezed juice;S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;S3: container is placed in progress microwave heating polyester in microwave reactor;S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains the multi-functional citrate of ethylene glycol after lye neutralisation treatment is then added.The volume production of the multi-functional citrate of ethylene glycol is able to achieve in the present invention using the method for the microwave heating technique production multi-functional citrate of ethylene glycol, and the time for generating the multi-functional citrate of ethylene glycol is shorter, compared to the production method of the multi-functional citrate of existing ethylene glycol, its production time can shorten at least one times, production cost is saved, and the multi-functional citrate stability of ethylene glycol produced is high.

Description

The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate
Technical field
The present invention relates to a kind of techniques for producing multi-functional citrate, specifically produce second two using microwave heating technique The technique that alcohol citrate is used for cosmetics.
Background technique
For ethylene glycol since molecular weight is low, property is active, can play the reaction such as esterification, etherificate, alcoholization, oxidation, acetal, dehydration, It is similar to ethyl alcohol, ester can be mainly generated with inorganic or organic acid reaction, general first only one hydroxyl reacts, through increasing temperature Degree, the sour dosage of increase etc., can make two hydroxyls all form ester.
At room temperature, citric acid is semi-transparent clear crystal or white particle or white crystalline powder to citric acid, odorless, Taste is extremely sour, micro- in wet air to have hygroscopy.It can exist in the form of no hydrate or monohydrate: citric acid When being crystallized from hot water, generate without hydrate;It is crystallized in cold water, generates monohydrate.It is heated to monohydrate at 78 DEG C It can decompose to obtain no hydrate.At 15 degrees Celsius, citric acid can also dissolve in dehydrated alcohol.
Ethylene glycol can also form ethylene glycol citrate in conjunction with citric acid, but be obtained according to research, existing production second The method of glycol citrate is unable to get stable ethylene glycol citrate and the time cycle is longer, generally requires 4-5h, nothing Method meets batch requirements.
Summary of the invention
The purpose of the present invention is to provide the works for utilizing microwave heating technique production ethylene glycol citrate to be used for cosmetics Skill, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate, comprising the following steps:
S1: fresh lemon is taken then to utilize squeezer that lemon is squeezed juice;
S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;
S3: container is placed in progress microwave heating polyester in microwave reactor;
S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains second after lye neutralisation treatment is then added The multi-functional citrate of glycol.
As a further solution of the present invention: in step sl, the lemon squeezing time is 2-2.5min.
As further scheme of the invention: in step s3, the microwave heating time is 1-2h.
As further scheme of the invention: in step s3, the microwave frequency is 2400-2500MHZ.
As further scheme of the invention: subtracting in the process of the vacuum distillation purification containing distilling apparatus, pumping Pressure device and pressure measuring unit.
As further scheme of the invention: the distilling apparatus includes cucurbit, kirschner still head, straight condensation Pipe, vacuum connect skirt and receiving flask.
Compared with prior art, the beneficial effects of the present invention are: producing ethylene glycol using microwave heating technique in the present invention The method of multi-functional citrate is able to achieve the volume production of the multi-functional citrate of ethylene glycol, and generates the multi-functional citric acid of ethylene glycol The time of ester is shorter, and compared to the production method of the multi-functional citrate of existing ethylene glycol, the production time can shorten at least one Times, production cost is saved, and the multi-functional citrate stability of ethylene glycol produced is high.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate, comprising the following steps:
S1: taking fresh lemon then to utilize squeezer that lemon is squeezed juice, and lemon squeezes the time as 2-2.5min;
S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;
S3: container, which is placed in progress microwave heating polyester, microwave heating time 1h, microwave frequency in microwave reactor, is 2500MHZ;
S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains second after lye neutralisation treatment is then added The multi-functional citrate of glycol is evaporated under reduced pressure in purification process containing distilling apparatus, pumping decompressor and pressure measuring unit, distillation Device includes that cucurbit, kirschner still head, straight cold finger, vacuum connect skirt and receiving flask.
Embodiment 2
The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate, comprising the following steps:
S1: taking fresh lemon then to utilize squeezer that lemon is squeezed juice, and lemon squeezes the time as 2-2.5min;
S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;
S3: container, which is placed in progress microwave heating polyester, microwave heating time 1.2h, microwave frequency in microwave reactor, is 2480MHZ;
S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains second after lye neutralisation treatment is then added The multi-functional citrate of glycol is evaporated under reduced pressure in purification process containing distilling apparatus, pumping decompressor and pressure measuring unit, distillation Device includes that cucurbit, kirschner still head, straight cold finger, vacuum connect skirt and receiving flask.
Embodiment 3
The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate, comprising the following steps:
S1: taking fresh lemon then to utilize squeezer that lemon is squeezed juice, and lemon squeezes the time as 2-2.5min;
S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;
S3: container, which is placed in progress microwave heating polyester, microwave heating time 1.4h, microwave frequency in microwave reactor, is 2460MHZ;
S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains second after lye neutralisation treatment is then added The multi-functional citrate of glycol is evaporated under reduced pressure in purification process containing distilling apparatus, pumping decompressor and pressure measuring unit, distillation Device includes that cucurbit, kirschner still head, straight cold finger, vacuum connect skirt and receiving flask.
Embodiment 4
The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate, comprising the following steps:
S1: taking fresh lemon then to utilize squeezer that lemon is squeezed juice, and lemon squeezes the time as 2-2.5min;
S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;
S3: container, which is placed in progress microwave heating polyester, microwave heating time 1.6h, microwave frequency in microwave reactor, is 2440MHZ;
S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains second after lye neutralisation treatment is then added The multi-functional citrate of glycol is evaporated under reduced pressure in purification process containing distilling apparatus, pumping decompressor and pressure measuring unit, distillation Device includes that cucurbit, kirschner still head, straight cold finger, vacuum connect skirt and receiving flask.
Embodiment 5
The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate, comprising the following steps:
S1: taking fresh lemon then to utilize squeezer that lemon is squeezed juice, and lemon squeezes the time as 2-2.5min;
S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;
S3: container, which is placed in progress microwave heating polyester, microwave heating time 1.8h, microwave frequency in microwave reactor, is 2420MHZ;
S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains second after lye neutralisation treatment is then added The multi-functional citrate of glycol is evaporated under reduced pressure in purification process containing distilling apparatus, pumping decompressor and pressure measuring unit, distillation Device includes that cucurbit, kirschner still head, straight cold finger, vacuum connect skirt and receiving flask.
Embodiment 6
The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate, comprising the following steps:
S1: taking fresh lemon then to utilize squeezer that lemon is squeezed juice, and lemon squeezes the time as 2-2.5min;
S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;
S3: container, which is placed in progress microwave heating polyester, microwave heating time 2h, microwave frequency in microwave reactor, is 2400MHZ;
S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains second after lye neutralisation treatment is then added The multi-functional citrate of glycol is evaporated under reduced pressure in purification process containing distilling apparatus, pumping decompressor and pressure measuring unit, distillation Device includes that cucurbit, kirschner still head, straight cold finger, vacuum connect skirt and receiving flask.
Conclusion: second two is able to achieve using the method for the microwave heating technique production multi-functional citrate of ethylene glycol in the present invention The volume production of the multi-functional citrate of alcohol, and the time for generating the multi-functional citrate of ethylene glycol is shorter, only needs 1-2h, compared to existing The multi-functional citrate of ethylene glycol production method, the production time can shorten at least one times, save production cost, Er Qiesheng The multi-functional citrate stability of the ethylene glycol of production is high.
The preferred embodiment of the patent is described in detail above, but this patent is not limited to above-mentioned embodiment party Formula within the knowledge of one of ordinary skill in the art can also be under the premise of not departing from this patent objective It makes a variety of changes.

Claims (6)

1. the technique for utilizing microwave heating technique production ethylene glycol citrate to be used for cosmetics, which is characterized in that including following Step:
S1: fresh lemon is taken then to utilize squeezer that lemon is squeezed juice;
S2: taking-up lemon juice is fitted into container and then dilute hydrochloric acid is added into container and is adjusted pH value to 6-6.5;
S3: container is placed in progress microwave heating polyester in microwave reactor;
S4: container is taken out from microwave reactor, and vacuum distillation purification process obtains second after lye neutralisation treatment is then added The multi-functional citrate of glycol.
2. the method according to claim 1 using the microwave heating technique production multi-functional citrate of ethylene glycol, special Sign is that in step sl, the lemon squeezing time is 2-2.5min.
3. the method according to claim 1 using the microwave heating technique production multi-functional citrate of ethylene glycol, special Sign is that in step s3, the microwave heating time is 1-2h.
4. the method according to claim 1 using the microwave heating technique production multi-functional citrate of ethylene glycol, special Sign is that in step s3, the microwave frequency is 2400-2500MHZ.
5. the method according to claim 1 using the microwave heating technique production multi-functional citrate of ethylene glycol, special Sign is, in step s 4, distilling apparatus, pumping decompressor and survey press fitting is contained in the process of the vacuum distillation purification It sets.
6. the method according to claim 5 using the microwave heating technique production multi-functional citrate of ethylene glycol, special Sign is, the distilling apparatus includes that cucurbit, kirschner still head, straight cold finger, vacuum connect skirt and receiving flask.
CN201811373365.3A 2018-11-19 2018-11-19 The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate Withdrawn CN109293505A (en)

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CN201811373365.3A CN109293505A (en) 2018-11-19 2018-11-19 The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate

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Application Number Priority Date Filing Date Title
CN201811373365.3A CN109293505A (en) 2018-11-19 2018-11-19 The technique for being used for cosmetics using microwave heating technique production ethylene glycol citrate

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112430186A (en) * 2019-08-24 2021-03-02 韦尔化学性能产品有限公司 Hydroxycarboxylic acid esters, process for their preparation and their use

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112430186A (en) * 2019-08-24 2021-03-02 韦尔化学性能产品有限公司 Hydroxycarboxylic acid esters, process for their preparation and their use
EP3786150A1 (en) 2019-08-24 2021-03-03 WeylChem Performance Products GmbH Hydroxycarboxylic acid esters, method for their preparation and their use
US11208372B2 (en) 2019-08-24 2021-12-28 Weylchem Performance Products, Gmbh Hydroxy carboxylic acid esters, manufacturing process thereof and use thereof

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