CN105037606A - Carbomer resin and preparing method thereof - Google Patents
Carbomer resin and preparing method thereof Download PDFInfo
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- CN105037606A CN105037606A CN201510544999.0A CN201510544999A CN105037606A CN 105037606 A CN105037606 A CN 105037606A CN 201510544999 A CN201510544999 A CN 201510544999A CN 105037606 A CN105037606 A CN 105037606A
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- Prior art keywords
- feed liquid
- carbomer
- carbomer resin
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- electron beam
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F216/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F216/12—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
Abstract
The invention discloses carbomer resin which comprises, by mass, 10-110 parts of carboxylic acid monomers, 0.01-1.5 parts of cross-linking agents, 10-1000 parts of water and 0.01-5.0 parts of other auxiliaries. The carboxylic acid monomers are carboxylic acids with alkenyl double-bond monomers. The cross-linking agents are provided with two or more double-bond monomers. The other auxiliaries are one or more of fatty alcohol benzene sulfonic acid sodium, fatty alcohol sodium sulfate, fatty alcohol polyoxyethylene ether, sulfate of fatty alcohol polyoxyethylene ether, hydrogen peroxide, peroxysulphate, EDTA, salt of the EDTA and the like. The invention further discloses a preparing method of the carbomer resin. According to the method for preparing the carbomer through an electron beam accelerator, no initiating agent is needed, the technology is simple and fast, and product performance is stable.
Description
Technical field
The present invention relates to a kind of carbomer resin and preparation method thereof, especially relate to a kind of novel method adopting electron beam irradiation to synthesize carbomer resin.
Background technology
Carbomer is a kind of important polyacrylic thickening material, is obtained by vinylformic acid (or methacrylic acid etc.) and allyl group cross-linking monomer generation chemical reaction.Its outward appearance is white powder, and energy water-soluble, ethanol, glycerine, second-order transition temperature is 100 ~ 105 DEG C.Containing 56% ~ 68% carboxyl in molecule, in slightly acidic, the pH of 0.5% water dispersion is 2.7 ~ 3.5.After making carboxylic ions after carbomer is neutralized, due to the repulsive interaction of negative charge, molecular chain disperse is stretched, in great swelling state, and tool viscosity.Gel after neutralization is insensitive to uviolizing, not temperature influence, does not support that bacterium mould increases.
Carbomer has excellent thickening, suspension and emulsifying effect, is widely used in medicine and cosmetic field.Only need the carbomer of small amount just can reach required stickiness, conventional amount used is 0.10%-0.50%, and has thickening and stable effect, thus can prepare the emulsion of the very wide and various flows sex change of viscosity scope, cream frost and gel-like product.And other thickening materials as all very high in the working concentration such as Mierocrystalline cellulose, xanthan gum (about 2%) just can reach effect same.Along with the raising day by day of standard of living, people more and more focus on the maintenance to the individual person, therefore day by day increase the demand of makeup and Medicines and Health Product, and this makes the Synthesis and applications of carbomer have broad prospects.
At present, producing carbomer is mostly react in organic solvent to form.
US Patent No. 2,798,053 1 kinds of carboxylic acid polyalcohols (Carboxylicpolymers), react and form in the middle of benzene, dimethylbenzene, tetraline, hexane, heptane, tetracol phenixin, monochloro methane, monochloroethane, trichloromethane equal solvent and mixture.
Chinese Patent Application No. is 201310453464.3 1 kinds of carbomers and preparation method thereof, adopts to react in the mixed solvent of ethyl acetate and hexanaphthene and normal hexane etc. to form.
Although adopt the organic solvent such as ethyl acetate, hexanaphthene of low toxicity to replace the solvent of the heavy poison such as benzene, but the dissolvent residual in material or inevitable existence, and the inputs of solvent-applied and solvent loss, solvent recuperation etc. all greatly increase carbomer products production cost, restrict the popularization of its market application.
Along with technical progress, the explained hereafter reaction medium preparing carbomer is also updating into low toxicity, micro-poison, nontoxic solvent.Chinese Patent Application No. is 201410010540.8 1 kinds of carbomers and preparation method thereof, and the reaction medium water of carbomer replaces the technique of a part of organic solvent to make the preparation of carbomer towards future development that is nontoxic, environmental protection.
The above-mentioned method preparing carbomer is all in a large amount of organic solvent, cause the polyreaction of carboxylic acid type monomer with chemical initiator, needs heating and control temperature, needs the reaction of long period to accumulate, finally synthesize carbomer resin.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of carbomer resin and preparation method thereof, is that one can not need initiator, and technique is simple and quick and product performance the are stable electron-beam accelerator that utilizes prepares the method for carbomer.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind of carbomer resin, comprises the raw material of following mass fraction: carboxylic acid type monomer 10 ~ 110 parts, linking agent 0.01 ~ 1.5 part, 10 ~ 1000 parts, water; Other auxiliary agent 0.01 ~ 5.0 part; Wherein, described carboxylic acid type monomer is for having thiazolinyl double bond monomer carboxylic-acid; Described linking agent is for having two or more double bond monomer; Other auxiliary agent described is one or more in fatty alcohol benzene sulfonic acid sodium salt, sodium alkyl sulfate, fatty alcohol-polyoxyethylene ether and vitriol thereof, hydrogen peroxide, persulphate, EDTA and its esters etc.
Aforesaid a kind of carbomer resin, is characterized in that: described carboxylic acid type monomer is at least one in vinylformic acid, methacrylic acid, β-crotonic acid.
Aforesaid a kind of carbomer resin, is characterized in that: described linking agent is at least one in thiazolinyl sucrose ether, pentaerythrite allyl ether, pentaerythritol acrylate, glyceryl acrylate.
A preparation method for carbomer resin as the aforementioned, is characterized in that: comprise the steps:
(1) carboxylic acid type monomer 10 ~ 110 parts, crosslinkers monomers 0.01 ~ 1.5 part, 10 ~ 1000 parts, water, other auxiliary agent 0.01 ~ 5.0 part are added in container, mix and obtain feed liquid to be polymerized, by this feed liquid certain speed by carrying out irradiation under electron beam, feed liquid rapid expansion becomes gelinite.
(2) the gelinite drying of step (1) is chopped into particle;
(3) granular powder of step (2) is broken into the carbomer resin of fine white powder
The preparation method of aforesaid a kind of carbomer resin, feature according to electron accelerator irradiation processing materials is: in described step (1), feed liquid is 0.5 m/min ~ 20 ms/min by the travelling speed of irradiation under electron beam, irradiation dose is 500Gy ~ 50kGy, and the thickness of feed liquid ensures be no more than 5 centimetres.
The preparation method of aforesaid a kind of carbomer resin, in step (1), the feed liquid of configuration to be loaded in PE poly-bag net air side by side and be placed in pallet, and the thickness of feed liquid is at below 50mm, pallet at the uniform velocity accepts irradiation by electron beam scanning window, obtains corresponding irradiation dose.
The preparation method of aforesaid a kind of carbomer resin, in step (1), the feed liquid of preparation is passed through the Pipeline transport of below D50 size, make the mouth of pipe close on electron beam irradiation scanning window place, adjustment certain flow rate makes feed liquid by electron beam scanning, obtains corresponding irradiation dose.
The invention has the beneficial effects as follows: utilize irradiating electron beams to cause the method for carboxylic acid type monomer's cross-linking polymerization synthesis carbomer resin, this polyreaction does not need thermal source, solve production control difficult point existing in prior art and production safety problem, and there is the advantage that control reactive mode is simple, production is quick, cost is low; The advantages such as can not need chemical initiator, the viscosity of gained carbomer resin is high, and molten water speed is fast, density is comparatively large, dust is little; Produce by industrial irradiation accelerator the object that high-octane electron beam irradiation material realizes materials synthesis, the feature of electron beam irradiation is that dose rate is high, and irradiation time is short, and absorption dose is accurate, simple operation.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
The invention provides a kind of carbomer resin, comprise the raw material of following mass fraction: carboxylic acid type monomer 10 ~ 110 parts, linking agent 0.01 ~ 1.5 part, 10 ~ 1000 parts, water; Other auxiliary agent 0.01 ~ 5.0 part; Wherein, described carboxylic acid type monomer is for having thiazolinyl double bond monomer carboxylic-acid; Described linking agent is for having two or more double bond monomer; Other auxiliary agent described is one or more in fatty alcohol benzene sulfonic acid sodium salt, sodium alkyl sulfate, fatty alcohol-polyoxyethylene ether and vitriol thereof, hydrogen peroxide, persulphate, EDTA and its esters etc.
Wherein, carboxylic acid type monomer is at least one in vinylformic acid, methacrylic acid, β-crotonic acid; Linking agent is at least one in thiazolinyl sucrose ether, pentaerythrite allyl ether, pentaerythritol acrylate, glyceryl acrylate etc.
Carboxylic acid type monomer through two or more double bond monomer crosslinked after, the space networks grating texture polycarboxylic acid resin exceeding molecular weight of low crosslinking degree can be formed.After this polycarboxylic acid resin powder is water-soluble, anionic carboxylic acid radical ion ionizes mutually, makes the grid exceeding molecular weight constantly in water, be expanded into full-bodied colloid.The proportioning of carboxylic acid type monomer and crosslinkers monomers, is comparatively applicable to the processing requirement preparing carbomer of electron beam irradiation.
Present invention also offers a kind of preparation method of carbomer resin, comprise the steps:
(1) carboxylic acid type monomer 10 ~ 110 parts, crosslinkers monomers 0.01 ~ 1.5 part, 10 ~ 1000 parts, water, other auxiliary agent 0.01 ~ 5.0 part are added in container, mix and obtain feed liquid to be polymerized, by this feed liquid certain speed by carrying out irradiation under electron beam, feed liquid rapid expansion becomes gelinite.
(2) the gelinite drying of step (1) is chopped into particle;
(3) granular powder of step (2) is broken into the carbomer resin of fine white powder
Wherein, in step (1), feed liquid is 0.5 m/min ~ 20 ms/min by the travelling speed of irradiation under electron beam, and irradiation dose is 500Gy ~ 50kGy, and the thickness of feed liquid ensures be no more than 5 centimetres.
Embodiment 1
A preferred version of carbomer resin preparation method of the present invention, comprises the steps:
(1) by Acrylic Acid Monomer 40 parts, thiazolinyl sucrose ether monomer 0.1 part, 50 parts, water; Sodium dodecylbenzene sulfonate 0.2 part adds in container, mixes and obtains feed liquid to be polymerized.
(2) feed liquid (1) prepared loads PE poly-bag, emptying air is placed in pallet, the thickness of feed liquid at below 50mm, pallet at the uniform velocity 5 meters/min by irradiation under beam intensity 10.3mA electron beam, make feed liquid absorption dose reach 15kGy, obtain the gel of carbomer resin;
(3) namely the oven dry of (2) gained gel, cutting, pulverizing are obtained finished product powder.
Utilize PE poly-bag packing feed liquid, can ensure that feed liquid makes carboxylic acid monomer obtain good reaction compartment under the environment of airtight emptying air, reactant is comparatively pure; The PE bag of packing is convenient to carrying transport and receives dosage continuously under irradiation apparatus.The effect of pallet is that carrying PE bag can the steady smooth irradiation by irradiator.
Embodiment 2
A preferred version of carbomer resin preparation method of the present invention, comprises the steps:
(1) by Acrylic Acid Monomer 50 parts, pentaerythrite allyl ether monomer 0.1 part, 70 parts, water; Sodium lauryl sulphate 0.1 part adds in container, mixes and obtains feed liquid to be polymerized.
(2) feed liquid (1) prepared, by pipeline adjustment flow velocity irradiation under 8 meters/min passes through beam intensity 9.3mA electron beam of D50, makes feed liquid absorption dose reach 18kGy, obtains the gel of carbomer;
(3) (2) gained gel dried, cut, pulverize, obtain carbomer resin powder.
Pipeline transport material below D5O size, guarantee material feed liquid at below 5cm, reaches the technical requirements of technology controlling and process and the stable of quality product by feed liquid thickness during irradiation scanning window ray.
In sum, a kind of carbomer resin provided by the invention and preparation method thereof is that one can not need initiator, and technique is simple and quick and product performance the are stable electron-beam accelerator that utilizes prepares the method for carbomer.
More than show and describe ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is by appending claims and equivalent circle thereof.
Claims (7)
1. a carbomer resin, is characterized in that: the raw material comprising following mass fraction: carboxylic acid type monomer 10 ~ 110 parts, linking agent 0.01 ~ 1.5 part, 10 ~ 1000 parts, water; Other auxiliary agent 0.01 ~ 5.0 part; Wherein, described carboxylic acid type monomer is for having thiazolinyl double bond monomer carboxylic-acid; Described linking agent is for having two or more double bond monomer; Other auxiliary agent described is one or more in fatty alcohol benzene sulfonic acid sodium salt, sodium alkyl sulfate, fatty alcohol-polyoxyethylene ether and vitriol thereof, hydrogen peroxide, persulphate, EDTA and its esters etc.
2.
according to claima kind of carbomer resin described in 1, is characterized in that: described carboxylic acid type monomer is at least one in vinylformic acid, methacrylic acid, β-crotonic acid.
3.
according to claima kind of carbomer resin described in 1, is characterized in that: described linking agent is at least one in thiazolinyl sucrose ether, pentaerythrite allyl ether, pentaerythritol acrylate, glyceryl acrylate.
4. one kind
as claimthe preparation method of the carbomer resin in 1-3 described in any one, is characterized in that: comprise the steps:
(1) carboxylic acid type monomer 10 ~ 110 parts, crosslinkers monomers 0.01 ~ 1.5 part, 10 ~ 1000 parts, water, other auxiliary agent 0.01 ~ 5.0 part are added in container, mix and obtain feed liquid to be polymerized, by this feed liquid with certain speed by carrying out irradiation under electron beam, feed liquid rapid expansion becomes gelinite.
5.(2) the gelinite drying of step (1) is chopped into particle;
(3) granular powder of step (2) is broken into the carbomer resin of fine white powder
according to claimthe preparation method of a kind of carbomer resin described in 4, it is characterized in that: in described step (1), feed liquid is 0.5 m/min ~ 20 ms/min by the travelling speed of irradiation under electron beam, irradiation dose is 500Gy ~ 50kGy, and the thickness of feed liquid ensures be no more than 5 centimetres.
6.
according to claimthe preparation method of a kind of carbomer resin described in 4, it is characterized in that: in step (1), the feed liquid of configuration to be loaded in PE poly-bag net air side by side and be placed in pallet, and the thickness of feed liquid is at below 50mm, pallet at the uniform velocity accepts irradiation by electron beam scanning window, obtains corresponding irradiation dose.
7.
according to claimthe preparation method of a kind of carbomer resin described in 4, it is characterized in that: the Pipeline transport in step (1), the feed liquid of preparation being passed through below D50 size, make the mouth of pipe close on electron beam irradiation scanning window place, adjustment certain flow rate makes feed liquid by electron beam scanning, obtains corresponding irradiation dose.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510544999.0A CN105037606A (en) | 2015-08-31 | 2015-08-31 | Carbomer resin and preparing method thereof |
| PCT/CN2015/098412 WO2017036001A1 (en) | 2015-08-31 | 2015-12-23 | Carbomer resin and preparation method therefor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510544999.0A CN105037606A (en) | 2015-08-31 | 2015-08-31 | Carbomer resin and preparing method thereof |
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| CN105037606A true CN105037606A (en) | 2015-11-11 |
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| CN201510544999.0A Pending CN105037606A (en) | 2015-08-31 | 2015-08-31 | Carbomer resin and preparing method thereof |
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| WO (1) | WO2017036001A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017036001A1 (en) * | 2015-08-31 | 2017-03-09 | 中广核达胜加速器技术有限公司 | Carbomer resin and preparation method therefor |
| CN106632803A (en) * | 2016-12-28 | 2017-05-10 | 贵州省欣紫鸿药用辅料有限公司 | Carbopol and preparation method thereof |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113896824B (en) * | 2020-07-06 | 2022-09-27 | 山东泰和水处理科技股份有限公司 | Synthetic method of polyacrylic acid crosslinked resin |
| CN113896823B (en) * | 2020-07-06 | 2022-09-27 | 山东泰和水处理科技股份有限公司 | Preparation method of polyacrylic acid crosslinked resin |
| CN114230708B (en) * | 2021-12-27 | 2023-01-03 | 湖北新德晟材料科技有限公司 | Carbomer and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2798053A (en) * | 1952-09-03 | 1957-07-02 | Goodrich Co B F | Carboxylic polymers |
| CN103755861A (en) * | 2014-01-09 | 2014-04-30 | 杭州拜善晟生物科技有限公司 | Carbomer and preparation method thereof |
| CN104448157A (en) * | 2014-11-25 | 2015-03-25 | 江苏达胜加速器制造有限公司 | Synthetic method for high-performance water-absorbent resin processed by electron beam irradiation |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000053719A (en) * | 1998-08-11 | 2000-02-22 | Toagosei Co Ltd | Production of acrylic polymer |
| CN101921359B (en) * | 2010-09-29 | 2012-04-18 | 湖南省原子能农业应用研究所 | Polyacrylic acid or copolymer thereof and preparation method of polyacrylate or copolymer salt thereof |
| CN103483491A (en) * | 2013-09-29 | 2014-01-01 | 清远市威仕泽科技孵化器有限公司 | Carbomer and preparation method thereof |
| CN104761673B (en) * | 2015-03-31 | 2017-11-14 | 四川理工学院 | A kind of carbomer and preparation method thereof |
| CN105037606A (en) * | 2015-08-31 | 2015-11-11 | 中广核达胜加速器技术有限公司 | Carbomer resin and preparing method thereof |
-
2015
- 2015-08-31 CN CN201510544999.0A patent/CN105037606A/en active Pending
- 2015-12-23 WO PCT/CN2015/098412 patent/WO2017036001A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2798053A (en) * | 1952-09-03 | 1957-07-02 | Goodrich Co B F | Carboxylic polymers |
| CN103755861A (en) * | 2014-01-09 | 2014-04-30 | 杭州拜善晟生物科技有限公司 | Carbomer and preparation method thereof |
| CN104448157A (en) * | 2014-11-25 | 2015-03-25 | 江苏达胜加速器制造有限公司 | Synthetic method for high-performance water-absorbent resin processed by electron beam irradiation |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017036001A1 (en) * | 2015-08-31 | 2017-03-09 | 中广核达胜加速器技术有限公司 | Carbomer resin and preparation method therefor |
| CN106632803A (en) * | 2016-12-28 | 2017-05-10 | 贵州省欣紫鸿药用辅料有限公司 | Carbopol and preparation method thereof |
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| WO2017036001A1 (en) | 2017-03-09 |
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