CN1569906A - Method for preparing powdered rubber through continuous coagulation - Google Patents
Method for preparing powdered rubber through continuous coagulation Download PDFInfo
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- CN1569906A CN1569906A CN 03145918 CN03145918A CN1569906A CN 1569906 A CN1569906 A CN 1569906A CN 03145918 CN03145918 CN 03145918 CN 03145918 A CN03145918 A CN 03145918A CN 1569906 A CN1569906 A CN 1569906A
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- latex
- mixing tank
- suspension
- separant
- mass parts
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 42
- 239000005060 rubber Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000015271 coagulation Effects 0.000 title abstract 2
- 238000005345 coagulation Methods 0.000 title abstract 2
- 238000002156 mixing Methods 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 35
- 239000000725 suspension Substances 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 229920000126 latex Polymers 0.000 claims abstract description 21
- 239000004816 latex Substances 0.000 claims abstract description 20
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000005642 Oleic acid Substances 0.000 claims abstract description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 4
- 238000005189 flocculation Methods 0.000 claims description 26
- 230000016615 flocculation Effects 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 150000002632 lipids Chemical class 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 239000000701 coagulant Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000008394 flocculating agent Substances 0.000 abstract 5
- 235000021355 Stearic acid Nutrition 0.000 abstract 1
- 235000014113 dietary fatty acids Nutrition 0.000 abstract 1
- 229930195729 fatty acid Natural products 0.000 abstract 1
- 239000000194 fatty acid Substances 0.000 abstract 1
- 150000004665 fatty acids Chemical class 0.000 abstract 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 abstract 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 abstract 1
- 235000021313 oleic acid Nutrition 0.000 abstract 1
- 239000008117 stearic acid Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 8
- 229940114930 potassium stearate Drugs 0.000 description 6
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229920000915 polyvinyl chloride Polymers 0.000 description 4
- 239000004800 polyvinyl chloride Substances 0.000 description 4
- 229940096992 potassium oleate Drugs 0.000 description 4
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 description 4
- 229920000459 Nitrile rubber Polymers 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- OCKPCBLVNKHBMX-UHFFFAOYSA-N butylbenzene Chemical compound CCCCC1=CC=CC=C1 OCKPCBLVNKHBMX-UHFFFAOYSA-N 0.000 description 2
- 238000005354 coacervation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000010092 rubber production Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 241001122126 Carex secta Species 0.000 description 1
- 229920013649 Paracril Polymers 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- -1 adding elasticity Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000002649 leather substitute Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention provides a method for preparing powdered rubber by continuous coagulation, which comprises the steps of mixing latex and a flocculating agent in a first mixer, then mixing the latex and the flocculating agent in a second mixer, and then mixing the latex and the flocculating agent in a third mixer, wherein the flocculating agent is water-soluble monovalent metal salt, the flocculating agent is water-soluble divalent or trivalent metal salt, and the isolating agent is monovalent metal salt of oleic acid, fatty acid and stearic acid; finally, the rubber powder enters a curing device for curing, and the obtained rubber powder suspension is subjected to post-treatment to obtain a rubber powder product.
Description
Technical field
The present invention relates to a kind of method for preparing powdered rubber, a kind of specifically continuous processing cohesion prepares the method for powdered rubber.
Background technology
Therefore powdered rubber is mainly used in resin modified because of having good consistency with the various kinds of resin blend.As in polyvinyl chloride, adding elasticity, water tolerance and the oil-proofness that a small amount of acrylonitrile-butadiene rubber powder can improve goods, also can improve the shock strength of the special-shaped extruded material of rigid polyvinyl chloride; Be used for the artificial leather product and can improve the leather surface cohesive force; Be used for the polyvinyl chloride calendered film, make film have better elasticity; Be used for the polyvinyl chloride electrical wire and cable goods, can improve its toughness and winter hardiness; Rubber powder and resol and usefulness have plastification etc.
Powdered rubber is compared with niggerhead, its rubber powder fine size, and during with other resin alloy, good dispersity, and can directly enter forcing machine, and make course of processing serialization, automatization, therefore have advantages such as easy to operate, energy-conservation.
The method for preparing at present rubber powder is a lot, and wherein coacervation gets most of the attention more.Chinese patent CN1031716 has invented a kind of single still and has been interrupted the method that substep condenses powder process end paracril, and this method technology is simple, cost is low, powder formation rate is high, isolation effect is good, separant content is low, filler-free, powder diameter are little.But this method has following shortcoming: the flocculation of latex, cohesion, slaking all in same still different times carry out, the operational cycle is long, be unsuitable for continuous mass production; Intermittent operation is difficult to realize the automatization control of production process.The method that a kind of tubular type is condensed powder process end rubber has continuously been invented at Chinese patents CN1266863A by Germany.The identical pipe of caliber before and after this method is used one section has two to three throttle mechanisms in the middle of the pipe, by first throttle mechanism, latex is mixed with filler, by second throttle mechanism, cohesion mixture is mixed with separant solution.Its shortcoming is: filler too many (50～100 mass parts), the powdered rubber particle is thick, and (particle diameter is 0.5～2mm), powder formation rate low (particle of many particle diameters greater than 2mm arranged).
Summary of the invention
The object of the present invention is to provide a kind of continuous processing cohesion to prepare the method for powdered rubber, to shorten the operational cycle, be easy to realize the automatization control of production process, and reduce the powder size of continuous processing powder process end rubber, improve the powder formation rate of serialization powder process end rubber.
For realizing the object of the invention, method of the present invention is: with latex through the dilution after, enter first mixing tank, mix with flocculant solution, obtain suspension through flocculation and enter second mixing tank, mix with coagulant solution, cohesion obtains rubber powder suspension and enters the 3rd mixing tank, with separant solution thorough mixing, the rubber powder suspension that is coated with separant enters ager, with 70～95 ℃ pyroprocessing 20～60 minutes, obtain work in-process powdered rubber suspension, this suspension promptly obtains the powdered rubber product through aftertreatment; Wherein flocculation agent is water-soluble univalent metal salt, and flocculation agent is water-soluble divalence, trivalent metal salt, and separant is oleic acid, lipid acid, stearic univalent metal salt.
The latex total solid substance massfraction that enters first mixing tank among the present invention is preferably 1%～20%, and the latex temperature is preferably 40 ℃～60 ℃, and the temperature control of mixing tank is preferably in 45 ℃～75 ℃.
Flocculation agent among the present invention is water-soluble univalent metal salt, is 100 mass parts (as follows) in latex (butt), and add-on is preferably 20～60 mass parts; Flocculation agent is water-soluble divalence, trivalent metal salt, and add-on is preferably 20～80 mass parts; Separant is oleic acid, lipid acid, stearic monovalent salt, and add-on is preferably 3～6 mass parts.
The same prior art of suspension aftertreatment of the present invention is promptly filtered, and washing, grinding are sieved and obtained the powdered rubber product.
Among the present invention, flocculation agent, flocculation agent, separant will mix in mixing tank.The conveying of material and mixing can be adopted various forms.As can being latex after dilution, enter first mixing tank, the flocculant solution that enters in this and side mixes, can produce flocculation, obtain suspension through flocculation and enter second mixing tank, the coagulant solution that enters in this and side mixes, and condenses, make the rubber particles of flocculation become real, moulding, obtain rubber powder suspension.This suspension enters the 3rd mixing tank, and with the abundant high efficient mixed of separant solution that the side enters, the rubber particles surface is coated by separant.The rubber powder suspension that is coated with separant enters ager, at this, with 70～95 ℃ pyroprocessing 20～60 minutes, obtains work in-process powdered rubber suspension.All use pump to come convey materials behind each section mixing tank, rely on the negative pressure that high-velocity fluid produced of pump delivery respectively flocculation agent, flocculation agent, separant to be sucked, and form the abundant high efficient mixed that turbulent flow guarantees material.
The present invention makes powdered rubber segmentation coacervation realize serialization, can improve the powder formation rate of continuous processing powder process end rubber, and powder particle is thin, and narrow diameter distribution has shortened the operational cycle greatly, has cancelled a large amount of weighting agents, can be used for various rubber latex condensation powderings; The flocculation of latex, cohesion, slaking are controlled in distinct device respectively simultaneously easily; Operate continuously can realize the automatization control of production process.The present invention has changed existing powdered rubber production technique, has promoted powdered rubber production, application and development.
Description of drawings
Fig. 1 prepares the powdered rubber process flow diagram for using a kind of continuous processing cohesion of the present invention, among the figure: 1-first mixing tank, 2-second mixing tank, 3-the 3rd mixing tank, 4-ager.
Embodiment
Embodiment 1
The nitrile rubber (NBR-40) that the total solid substance massfraction is 15%, flow is 5.0Kg/h and flow are that the flocculation agent NaCl solution (massfraction is 15%) of 2.0Kg/h mixes in first mixing tank, temperature is 60 ℃, and this mixed solution is the flocculation agent MgSO of 1.2Kg/h with flow in second mixing tank
4Solution (massfraction is 25%) mixes, and temperature is 60 ℃.The gained powder suspension is that separant potassium oleate and potassium stearate (potassium oleate is 2: 1 with the mass ratio of the potassium stearate) mixing solutions (massfraction is 8%) of 0.46Kg/h mixes with flow in the 3rd mixing tank, temperature is 70 ℃, enter ager through isolated powdered rubber suspension, 85 ℃ of following slakings 30 minutes, the powdered rubber suspension that obtains is sent to dehydration, drying, obtain the powdered rubber product, powder diameter: 0.4～0.5mm, powder formation rate is more than 95%.
Embodiment 2:
The total solid substance massfraction is 12%, flow is 6.0Kg/h, and treated SBR-1500 latex, with flow is that the flocculation agent KCl solution (massfraction is 25%) of 1.7Kg/h is in mixing in first mixing tank under 55 ℃, entering then in second mixing tank, is the flocculation agent CaCl of 1.7Kg/h with flow down at 60 ℃
2Solution (massfraction is 25%) mixes.The suspension that obtains enters the 3rd mixing tank, is that separant potassium oleate and potassium stearate (potassium oleate is 1: 1 with the mass ratio of the potassium stearate) mixing solutions (massfraction is 8%) of 0.36Kg/h mixes with flow, and the suspension that obtains enters ager.90 ℃ of following slakings 20 minutes, the powdered rubber suspension that obtains is sent to dehydration, and the powder after the dehydration enters the moisture eliminator drying after disperseing, obtain powder butylbenzene product, and particle diameter is 0.4～0.5mm, and powder formation rate is more than 95%.
Embodiment 3:
The total solid substance massfraction is 10%, flow is 6.0Kg/h, and treated polybutadiene latex, with flow is that the flocculation agent NaCl solution (massfraction is 25%) of 1.2Kg/h is in mixing in first mixing tank under 50 ℃, entering then in second mixing tank, is the flocculation agent MgCl of 1.8Kg/h with flow down at 55 ℃
2Solution (massfraction is 25%) mixes.The suspension that obtains enters the 3rd mixing tank, is that separant lipid acid potassium and potassium stearate (lipid acid potassium is 3: 1 with the mass ratio of the potassium stearate) mixing solutions (massfraction is 8%) of 0.23Kg/h mixes with flow, and the suspension that obtains enters ager.95 ℃ of following slakings 25 minutes, the powdered rubber suspension that obtains is sent to dehydration, and the powder after the dehydration enters the moisture eliminator drying after disperseing, obtain powder polyhutadiene product, and particle diameter is 0.4～0.5mm, and powder formation rate is more than 95%.
Annotate: powder formation rate refers to account for input latex (butt) mass percent less than the particle mass of 1.2mm.
Claims (9)
1. a continuous processing is condensed the method for preparing powdered rubber, with latex through the dilution after, enter first mixing tank, with the flocculant solution thorough mixing, obtain suspension through flocculation and enter second mixing tank, with the coagulant solution thorough mixing, cohesion obtains rubber powder suspension and enters the 3rd mixing tank, with separant solution thorough mixing, the rubber powder suspension that is coated with separant enters ager, with 70～95 ℃ pyroprocessing 20～60 minutes, obtain work in-process powdered rubber suspension, this suspension promptly obtains the powdered rubber product through aftertreatment; Wherein flocculation agent is water-soluble univalent metal salt, and flocculation agent is water-soluble divalence, trivalent metal salt, and separant is oleic acid, lipid acid, stearic univalent metal salt.
2. method according to claim 1, the latex total solid substance massfraction that it is characterized in that entering first mixing tank is 1%～20%.
3. method according to claim 1, the latex temperature that it is characterized in that entering first mixing tank is 40 ℃～60 ℃.
4. method according to claim 1, the temperature that it is characterized in that mixing tank are 45 ℃～75 ℃.
5. method according to claim 1 is characterized in that the butt in latex is 100 mass parts, and flocculant addition is 20～60 mass parts.
6. method according to claim 1 is characterized in that the butt in latex is 100 mass parts, and the flocculation agent add-on is 20～80 mass parts.
7. method according to claim 1 is characterized in that the butt in latex is 100 mass parts, and the separant add-on is 3～6 mass parts.
8. method according to claim 1 is characterized in that aftertreatment refers to that work in-process powdered rubber suspension filters, and washing, grinding are sieved.
9. according to the described any method of claim 1 to 8, it is characterized in that all using pump to come convey materials behind each section mixing tank, rely on the negative pressure that high-velocity fluid produced of pump delivery respectively flocculation agent, flocculation agent, separant to be sucked, and form the abundant high efficient mixed that turbulent flow guarantees material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03145918 CN1267458C (en) | 2003-07-17 | 2003-07-17 | Method for preparing powdered rubber through continuous coagulation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03145918 CN1267458C (en) | 2003-07-17 | 2003-07-17 | Method for preparing powdered rubber through continuous coagulation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1569906A true CN1569906A (en) | 2005-01-26 |
| CN1267458C CN1267458C (en) | 2006-08-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03145918 Expired - Fee Related CN1267458C (en) | 2003-07-17 | 2003-07-17 | Method for preparing powdered rubber through continuous coagulation |
Country Status (1)
| Country | Link |
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| CN (1) | CN1267458C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153707A (en) * | 2011-02-18 | 2011-08-17 | 万达集团股份有限公司 | Method for preparing large-particle-size high-impact-resistance MBS resin |
| CN102190741A (en) * | 2010-03-19 | 2011-09-21 | 中国石油天然气股份有限公司 | Method for coagulating rubber latex |
| CN102453288A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工股份有限公司 | Toughened PVC (polyvinyl chloride) resin with high apparent density and preparation method thereof |
| CN103159611A (en) * | 2011-12-15 | 2013-06-19 | 中国石油天然气股份有限公司 | Preparation method of flame-retardant separant |
| CN103804530A (en) * | 2012-11-14 | 2014-05-21 | 中国石油天然气股份有限公司 | Preparation method of modified powdered styrene butadiene rubber |
| CN103804735A (en) * | 2012-11-14 | 2014-05-21 | 中国石油天然气股份有限公司 | Preparation method of modified oil-extended powder styrene-butadiene rubber |
| CN104710547A (en) * | 2013-12-17 | 2015-06-17 | 北方华锦化学工业集团有限公司 | Agglomeration method of polybutadiene latex used for acrylonitrile butadiene styrene (ABS) resin |
| EP3604397A4 (en) * | 2017-03-28 | 2020-11-18 | Zeon Corporation | Method for producing carboxyl-group-containing nitrile rubber |
-
2003
- 2003-07-17 CN CN 03145918 patent/CN1267458C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190741A (en) * | 2010-03-19 | 2011-09-21 | 中国石油天然气股份有限公司 | Method for coagulating rubber latex |
| CN102453288A (en) * | 2010-10-22 | 2012-05-16 | 中国石油化工股份有限公司 | Toughened PVC (polyvinyl chloride) resin with high apparent density and preparation method thereof |
| CN102453288B (en) * | 2010-10-22 | 2013-06-12 | 中国石油化工股份有限公司 | Toughened PVC (polyvinyl chloride) resin with high apparent density and preparation method thereof |
| CN102153707A (en) * | 2011-02-18 | 2011-08-17 | 万达集团股份有限公司 | Method for preparing large-particle-size high-impact-resistance MBS resin |
| CN103159611A (en) * | 2011-12-15 | 2013-06-19 | 中国石油天然气股份有限公司 | Preparation method of flame-retardant separant |
| CN103159611B (en) * | 2011-12-15 | 2014-12-24 | 中国石油天然气股份有限公司 | Preparation method of flame-retardant separant |
| CN103804530A (en) * | 2012-11-14 | 2014-05-21 | 中国石油天然气股份有限公司 | Preparation method of modified powdered styrene butadiene rubber |
| CN103804735A (en) * | 2012-11-14 | 2014-05-21 | 中国石油天然气股份有限公司 | Preparation method of modified oil-extended powder styrene-butadiene rubber |
| CN103804735B (en) * | 2012-11-14 | 2016-06-08 | 中国石油天然气股份有限公司 | Preparation method of modified oil-extended powder styrene-butadiene rubber |
| CN103804530B (en) * | 2012-11-14 | 2016-08-03 | 中国石油天然气股份有限公司 | Preparation method of modified powdered styrene butadiene rubber |
| CN104710547A (en) * | 2013-12-17 | 2015-06-17 | 北方华锦化学工业集团有限公司 | Agglomeration method of polybutadiene latex used for acrylonitrile butadiene styrene (ABS) resin |
| EP3604397A4 (en) * | 2017-03-28 | 2020-11-18 | Zeon Corporation | Method for producing carboxyl-group-containing nitrile rubber |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1267458C (en) | 2006-08-02 |
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Granted publication date: 20060802 Termination date: 20210717 |