CN101481429A - Industrial production method for producing chlorinated rubber by aqueous phase suspension - Google Patents
Industrial production method for producing chlorinated rubber by aqueous phase suspension Download PDFInfo
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- CN101481429A CN101481429A CNA2009100956264A CN200910095626A CN101481429A CN 101481429 A CN101481429 A CN 101481429A CN A2009100956264 A CNA2009100956264 A CN A2009100956264A CN 200910095626 A CN200910095626 A CN 200910095626A CN 101481429 A CN101481429 A CN 101481429A
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Abstract
The invention discloses an industrialized production method for preparing chlorinated rubber by an aqueous-phase suspension method. T method comprises the following steps: clear water and natural latex are added to a glass-lined reaction kettle with an agitator on the premise of aqueous-phase suspension state of the natural latex, then a nonionic surfactant, a cationic surfactant, and a peroxide initiator are added to the kettle respectively. The method is technologically characterized by introducing chlorine for a chlorination reaction under ultraviolet lamp radiation while stirring when the temperature is controlled below 10 DEG C, heating to 10-40 DEG C when the chlorine content reaches 30% of a theoretical value, introducing the rest chlorine when the chlorine content reaches 80% and the temperature is not higher than 130 DEG C, keeping the temperature for 0.5-2h after completion of the reaction, then replacing the residual chlorine in the kettle with clean air, and heating to 140 DEG C to degrade molecular weight of the chlorinated rubber; and then washing with water to deacidify, neutralizing, dehydrating and drying to obtain the chlorinated rubber finished product. The method has the advantages of no pollution to the surrounding environment, short reaction time, lower cost and considerable economic benefit.
Description
Technical field
The present invention relates to the macromolecule chemical industry field, is a kind of under the aqueous-phase suspending state, carries out chlorination reaction with natural emulsion, makes the industrialized preparing process of chlorinated rubber, and the chlorinated rubber finished product that makes with present method.
Background technology
Chlorinated rubber all carries out chlorination reaction with solvent method and produces, because solvent method cost height, and some have residual solvent in harm and volatile matter contaminate environment and the product as the tetracol phenixin equal solvent to the person and make defectives such as purposes is restricted.
Bibliographical information is arranged both at home and abroad though water phase suspension is produced chlorinated rubber, show, domesticly still be in the research trial stage according to looking into new data; Though there is 800 tons/year industrial production device in deer island factory of the electrochemical company of the external Japanese rising sun, production method of the present invention has very big difference (China Chemical Information Center's " novelty assessment report " numbering: 2000-086) with it.
Summary of the invention
A kind of industrialized preparing process of method of chlorinated rubber by adopting water phase suspension, this method are to be medium with the water purification with natural emulsion under the aqueous-phase suspending state, are raw material with the natural emulsion, and raw materials used is the natural emulsion of emulsion form.Then adding earlier with a kind of in the nonionogenic tenside in raw material is emulsification promotor, as polyoxyethylene nonylphenol ether, alkyl phenolic group Soxylat A 25-7, Viscotrol C-Soxylat A 25-7, C12-C14 alkanoic acid diethanolamine etc.; Add-on is 0.5~3% of a latex weight.Adding then with a kind of in the cats product serves as to disperse separant, as 18-alkyl dimethyl benzyl ammonium chloride, 14-alkyl dimethyl benzyl ammonium chloride, alkyl trimethyl ammonium chloride, cocounut oil alkyl front three ammonium chloride, alkyl trimethyl sulfuric acid formicester ammonium etc.; Its add-on also is 0.5~3% of a latex weight.Add superoxide again and do to activate initiator, as dilauroyl peroxide, Diisopropyl azodicarboxylate, dibenzoyl peroxide etc.Add-on is 1~5% of a latex weight.Add emulsification promotor sequentially, disperse separant and activate initiator, make solution be suspension milkiness state through stirring, under the irradiation of ultraviolet, divide three temperature sections to feed chlorine, in same glassed steel reaction vessels, finish chlorination reaction continuously, reaction is warming up to 140 ℃ after ending again, the molecular weight of degraded chlorinated rubber is with the product of preparation different viscosity, again through technological processs such as washing depickling, neutralization, dehydration, dryings, finally making chlorinity is between 60~70%, the finely powdered that is white in color finished product.This method at first adds water purification and raw material in reactor, water purification is for filtering back clean process water, deionized water, distilled water, and its weight is 10~20 times of natural emulsion.In the glassed steel reaction vessels that stirs to band, add water purification and natural emulsion, at first add nonionogenic tenside then, the combination solution that adds cats product is again put in the glassed steel reaction vessels after fully stirring, and is aqueous-phase suspending emulsion form preferably through stirring.Under the irradiation of ultraviolet light, feed chlorine and carry out chlorination reaction.The power of UV-lamp is between 500~3000W, and wavelength is 260~360nm.Feed chlorine and divide three temperature sections to carry out chlorination reaction, the fs temperature is below 10 ℃, and chlorine feeding amount is for feeding 30% of total amount; The subordinate phase temperature is at 10~40 ℃, and chlorine feeding amount is for feeding 50% of total amount; At 40~130 ℃, feed remaining chlorine in the phase III temperature.The total amount that feeds chlorine is 3~5 times of natural emulsion weight, adds peroxide initiator at last; Each temperature section feeds the weight and the ratio of chlorine and is controlled by measure monitor the back as calculated.Its technical essential is that temperature is controlled at below 10 ℃ under the irradiation of stirring and ultraviolet light, feeds chlorine and carries out chlorination reaction; When chlorine feeding amount reach should the feeding amount 30% the time, heat up and enter subordinate phase, temperature is controlled at 10~40 ℃, when chlorine feeding amount reach should the feeding amount 80% the time, heat up and enter the phase III, before top temperature is no more than 130 ℃, feed remaining chlorine; After reaction finished, insulation earlier 0.5~2 hour was driven remaining chlorine in the still away with uncontaminated air again, and is warming up to 140 ℃, the molecular weight of degraded chlorinated rubber, and purpose is the chlorinated rubber finished product that can prepare different viscosity according to user's requirement.Through washing depickling, neutralization, dehydration, drying, promptly obtain the chlorinated rubber finished product again, the finished product are the white fine powder shape solid of chlorinity 65%.
Chlorinity of the present invention is up to 60~75%, and can fully dissolving in organic solvents such as toluene, dimethylbenzene, and good with other resin compatibilities, it is limpid that solution is.Reaction whole process of the present invention is to finish under the aqueous-phase suspending state of same reactor, and surrounding enviroment are not polluted.And be that the reaction times is short, be convenient to operation, adapt to scale production, cost is lower, and economic benefit is considerable.
Embodiment
The invention will be further described by the following examples.For embodiment, be the example that actually operating is verified in mass-producing trial production.Therefore, be easy to be grasped by those skilled in the art.Change as make some on basis of the present invention, its essence does not exceed the scope that the present invention includes.Described embodiment only makes an explanation to the present invention, is not that the present invention is made restriction.
Embodiment
In the glassed steel reaction vessels that 2000 liters of bands stir, add water purification 1500Kg and natural emulsion 100Kg, at first add nonionogenic tenside agent 500g then, the combination solution that adds cats product 500g again is after fully stirring, put in the glassed steel reaction vessels, add peroxide initiator 1000g at last.Under the irradiation of stirring and ultraviolet light, temperature is controlled at below 10 ℃, feeds chlorine and carries out chlorination reaction.When chlorine feeding amount reach should the feeding amount 30% the time, heat up and enter subordinate phase, temperature is controlled at 10~40 ℃, when chlorine feeding amount reach should the feeding amount 80% the time, heat up and enter the phase III, before top temperature is no more than 130 ℃, feed remaining chlorine.The chlorine total amount that feeds is 360Kg.After reaction finished, insulation earlier 1.5 hours was driven remaining chlorine in the still away with uncontaminated air again, and is warming up to 140 ℃, the molecular weight of degraded chlorinated rubber.Through washing depickling, neutralization, dehydration, drying, promptly obtain the chlorinated rubber finished product again, the finished product are the white fine powder shape solid of chlorinity 65%.
Claims (1)
1, a kind of industrialized preparing process of method of chlorinated rubber by adopting water phase suspension, this method is to be medium with the water purification with natural emulsion under the aqueous-phase suspending state, with the natural emulsion is raw material, add emulsification promotor sequentially, disperse separant and activate initiator, in the glassed steel reaction vessels that band stirs, add water purification and natural emulsion, at first add nonionogenic tenside then, the combination solution that adds cats product again is after fully stirring, put in the glassed steel reaction vessels, add peroxide initiator at last; It is characterized in that temperature is controlled at below 10 ℃ under the irradiation of stirring and ultraviolet light, feed chlorine and carry out chlorination reaction; When chlorine feeding amount reach should the feeding amount 30% the time, heat up and enter subordinate phase, temperature is controlled at 10~40 ℃, when chlorine feeding amount reach should the feeding amount 80% the time, heat up and enter the phase III, before top temperature is no more than 130 ℃, feed remaining chlorine; After reaction finished, insulation earlier 0.5~2 hour was driven remaining chlorine in the still away with uncontaminated air again, and is warming up to 140 ℃, the molecular weight of degraded chlorinated rubber; Through washing depickling, neutralization, dehydration, drying, promptly obtain the chlorinated rubber finished product again, the finished product are the white fine powder shape solid of chlorinity 65%.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102174126A (en) * | 2011-03-07 | 2011-09-07 | 福建师范大学 | Method for preparing chlorinated rubber by water phase photocatalysis |
CN102250262A (en) * | 2010-12-28 | 2011-11-23 | 广东海洋大学 | Method for preparing viscosity controllable chlorinated natural rubber |
CN105418809A (en) * | 2016-01-05 | 2016-03-23 | 临沂奥星化工有限公司 | Preparation method of chlorinated rubber |
CN108912430A (en) * | 2018-07-23 | 2018-11-30 | 宁波昊鑫裕隆新材料有限公司 | A kind of chlorinated rubber and preparation method and purposes of nanometer additive and Sodium Allyl Sulfonate modified synergic |
CN109824804A (en) * | 2019-01-31 | 2019-05-31 | 杭州科利化工股份有限公司 | A kind of preparation method of chlorinated polyethylene rubber |
-
2009
- 2009-01-13 CN CNA2009100956264A patent/CN101481429A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102250262A (en) * | 2010-12-28 | 2011-11-23 | 广东海洋大学 | Method for preparing viscosity controllable chlorinated natural rubber |
CN102174126A (en) * | 2011-03-07 | 2011-09-07 | 福建师范大学 | Method for preparing chlorinated rubber by water phase photocatalysis |
CN102174126B (en) * | 2011-03-07 | 2012-11-14 | 福建师范大学 | Method for preparing chlorinated rubber by water phase photocatalysis |
CN105418809A (en) * | 2016-01-05 | 2016-03-23 | 临沂奥星化工有限公司 | Preparation method of chlorinated rubber |
CN108912430A (en) * | 2018-07-23 | 2018-11-30 | 宁波昊鑫裕隆新材料有限公司 | A kind of chlorinated rubber and preparation method and purposes of nanometer additive and Sodium Allyl Sulfonate modified synergic |
CN108912430B (en) * | 2018-07-23 | 2020-09-29 | 宁波昊鑫裕隆新材料有限公司 | Chlorinated rubber synergistically modified by nano additive and sodium allylsulfonate, preparation method and application |
CN109824804A (en) * | 2019-01-31 | 2019-05-31 | 杭州科利化工股份有限公司 | A kind of preparation method of chlorinated polyethylene rubber |
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