CN102070789B - Preparation method of powder rubber - Google Patents
Preparation method of powder rubber Download PDFInfo
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- CN102070789B CN102070789B CN200910238563A CN200910238563A CN102070789B CN 102070789 B CN102070789 B CN 102070789B CN 200910238563 A CN200910238563 A CN 200910238563A CN 200910238563 A CN200910238563 A CN 200910238563A CN 102070789 B CN102070789 B CN 102070789B
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Abstract
The invention provides a preparation method of powder rubber, and the preparation method comprises the following steps: adding a separant into rubber latex, and evenly mixing; while stirring, adding a coagulant to coagulate at minus 30-minus 5 DEG C; and separating, dehydrating and drying to obtain the powder rubber. In the invention, the rubber latex directly coagulates into powder rubber at low temperature; the coagulation process is simple and stable, and can be easily controlled; and the rubber powder has the advantages of high yield, and small and uniform particle size, and can ensure the subsequent procedure to be smooth.
Description
Technical field
The present invention relates to a kind of preparation method of powdered rubber, be specifically related to the powdered rubber preparation method of the direct condensation powdering of a kind of low temperature.
Background technology
At present, the method for preparing powdered rubber mainly contains: mechanical crushing method, spray-drying process and cohesion coating method etc.Wherein mechanical crushing method is to be raw material with the solid rubber, carries out normal temperature or freezing and pulverizing, adopts this method, and energy consumption is big, and yield is low, and powder is thick, and particle is irregular, and production cost is high.Spray-drying process exists the release agent consumption big, and nonrubber composition such as emulsifying agent a large amount of shortcomings such as residual in drying influence product performance in the latex.And cohesion coating method processing unit is simple relatively, energy consumption is low, and used coating mainly contains: inorganics (as: water glass, WHITE CARBON BLACK and CaCO
3, talcum powder etc.), starch xanthogenic acid ester, macromolecule resin etc.; Wherein adopt the inorganics isolation method; The inorganics large usage quantity, owing to be physical adsorption between inorganic particles and the rubber surface, inorganic particles is easy to come off in storage and transport process simultaneously; Cause adhesion and inorganic particles dust from flying between the rubber particles; Be unfavorable for prolonged preservation, in the occasion that the ash oontent in the rubber is had strict demand, this method is inapplicable; And, have a strong impact on the quality of powdered rubber product with starch xanthate is easy mouldy between the shelf lives as the powdered rubber of coating preparation, xanthochromia is aging.
Mention in the CN200410046023.2 invention and adopt direct coacervation to become the powder technology to prepare the method for powdered rubber; Its preparation method is that rubber latex is joined in the aqueous solution that contains flocculation agent; In the condensation powdering process, add the organic carboxyl acid alkali metal soap then, obtain the powdered rubber product at last.This method does not add qualification as if the pH to coacervated system or latex; Agglomeration process temperature too high (40～80 ℃), latex can be very unstable in agglomeration process, very easily caking; Cause powder formation rate low even can not become powder, and subsequent technique is like dehydration, the drying very difficulty that also becomes.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, adopt the direct condensation powdering prepared of low temperature powdered rubber, agglomeration process is simple, stable, easy to control, and the gained powder formation rate is high, and particle diameter is little and even, and can guarantee that subsequent handling is smooth.
The preparation method of powdered rubber of the present invention is: separant is joined in the rubber latex, fully mix, under agitation condition, add the flocculation agent cohesion, condensation temperature is-30～-5 ℃, makes powdered rubber through separation, dehydration, drying.
Rubber latex of the present invention can be a natural rubber latex; Also can be negatively charged ion or nonionic emulsifying agent synthetic latex, the independent polymkeric substance of conjugated diolefine hydrocarbon compound that polymerization makes like conventional emulsion, content of polybutadiene rubber latex, X 050 latex etc.; The binary or the terpolymer of vinyl compounds such as conjugated diolefine hydrocarbon compound and vinylbenzene, vinyl cyanide, vinylformic acid, methylacrylic acid are like styrene butadiene rubber latex, paracril latex, carboxy nitrile rubber latex, carboxylic styrene-butadiene rubber latex etc.
Condensation temperature of the present invention is preferably-15～-5 ℃.
Separant of the present invention can be in potassium stearate, StNa, potassium oleate, sodium oleate, synthetic fatty acid potassium, the sodium fat synthesis one or more; Concentration is 16%～22% (weight percentage); Weight by dry rubber, per 100 mass parts latex, add-on is 0.1～20 part.
Flocculation agent described in the present invention can be univalent metal salt, divalent metal salt, also can be trivalent metal salt.For example NaCl, KCl, CaCl
2, MgSO
4, in the alum one or more.Described flocculation agent uses with aqueous solution form, and volumetric concentration is 2%～25%, is preferably 5%～20%, weight by dry rubber, and per 100 mass parts latex, add-on is 0.1～25 part, is preferably 3～15 parts.
Among the present invention rubber latex and separant thorough mixing are stirred; Directly add the flocculation agent cohesion at low temperatures, because at low temperatures, the probability that latex particle collides each other is little; The chance of coacervating large particle is also few; Therefore agglomeration process is stable, and compole is short when becoming powder, and resulting rubber powder is also thinner.
Separant of the present invention and flocculation agent add-on are less, in agglomeration process, need not to add in addition separant and just can reach isolation effect preferably, and powderised process stabilizing, reliable need not the slaking that heats up after the powdered rubber cohesion is accomplished, and is easy and simple to handle, saves operation.
Adopt the inventive method, make the powder formation rate of rubber latex can reach more than 99%, gained powdered rubber particle is thin, narrow diameter distribution.
Adopt the prepared powdered rubber performance of the inventive method similar with block colloidality ability, and good fluidity, shelf-stable, prevented from caking.
Embodiment
Through concrete embodiment the preparation method of powdered rubber of the present invention is done further explain below.
The rubber latex that is adopted among the embodiment is described below:
(A) styrene butadiene rubber latex (to call SBR in the following text): styrene butadiene rubber latex SBR-1500, SBR-1502, SBR-1712 that CNPC's Lanzhou Petrochemical is produced.
(B) paracril latex (to call NBR in the following text): the DN631 latex that contains carboxyl functional group that CNPC's Lanzhou Petrochemical is produced, low gel and the N32 latex of low mooney viscosity and the N41 latex of high Mooney viscosity.
(C) content of polybutadiene rubber latex (to call BR in the following text): the polybutadiene latex that CNPC's Lanzhou Petrochemical is produced.
(D) natural rubber latex (to call CR in the following text): the natural rubber latex that Yunnan tree elastomer industry limited-liability company produces.
Embodiment 1
Get the SBR-1500 latex of the dried glue of 500g, the adding mass concentration is 18.2% Triple Pressed Stearic Acid potash soap 165g.Mix, be cooled to-28 ℃, the adding volumetric concentration is 10% MgSO
4Solution 1250ml condenses, and last warp filters, washing is drying to obtain powder SBR-1500 rubber product, the following powder formation rate 99.5% of 0.4mm.
Comparative Examples 1
Get the SBR-1500 latex of the dried glue of 500g, the adding mass concentration is 18.2% Triple Pressed Stearic Acid potash soap 165g.Mix, be warming up to 40 ℃, the adding volumetric concentration is 10% MgSO
4Solution 1250ml condenses, and last warp filters, washing is drying to obtain powder SBR-1500 rubber product, the following powder formation rate 92.3% of 0.9mm.
Embodiment 2
Get the SBR-1502 latex of the dried glue of 450g, the adding mass concentration is 21% synthetic fatty acid potassium 43g.Mix, be cooled to-20 ℃, the adding volumetric concentration is 5% CaCl
2Solution 720ml condenses, and last warp filters, washing is drying to obtain powder SBR-1502 product, the following powder formation rate 99.2% of 0.35mm.
Comparative Examples 2
Get the SBR-1502 latex of the dried glue of 450g, the adding mass concentration is 21% synthetic fatty acid potassium 43g.Mix, be warming up to 60 ℃, the adding volumetric concentration is 5% CaCl
2Solution 720ml condenses, and last warp filters, washing is drying to obtain powder SBR-1502 product, the following powder formation rate 53.8% of 1.5mm.
Embodiment 3
Get the SBR-1712 latex of the dried glue of 400g, the adding mass concentration is 19.8% potassium oleate 30.3g.Mix; Be cooled to-15 ℃; Adding volumetric concentration then respectively and be 25% NaCl 168ml and volumetric concentration is that 3%CaCl2 solution 1000ml condenses, last through filter, washing is drying to obtain powder SBR-1712 product, the following powder formation rate 99.6% of 0.3mm.
Comparative Examples 3
Get the SBR-1712 latex of the dried glue of 400g, the adding mass concentration is 19.8% potassium oleate 30.3g.Mix, under 10 ℃ of conditions, adding volumetric concentration respectively and be 25% NaCl solution 168ml and volumetric concentration is 3%CaCl
2Solution 100ml, powder formation rate are 82.1%.
Embodiment 4
Get the N32 latex of the dried glue of 550g, add mass concentration and be 21.3% potassium stearate 158g and concentration and be 17.9% sodium fat synthesis 119g.Mix, be cooled to-10 ℃, add volumetric concentration then respectively and be 15% NaCl300ml and volumetric concentration and be 10% MgSO
4Solution 429ml condenses, and last warp filters, washing is drying to obtain powder N32 product, the following powder formation rate 99.1% of 0.3mm.
Embodiment 5
Get the DN631 latex of the dried glue of 380g, add mass concentration and be 18.8% sodium oleate 143g and concentration and be 16.5% potassium stearate 114g.Mix, be cooled to-5 ℃, add volumetric concentration then and be 20% alum liquor 228ml and condense, last through filter, washing is drying to obtain powder DN631 product, the following powder formation rate 99.6% of 0.4mm.
Embodiment 6
Get the N41 latex of the dried glue of 460g, add mass concentration and be 21.8% sodium oleate 138g and concentration and be 17.2% sodium fat synthesis 254g.Mix; Be cooled to-12 ℃; Add volumetric concentration then respectively and be 25% NaCl solution 168ml and volumetric concentration and be 18% alum liquor 262ml and condense, last through filter, washing is drying to obtain powder N41 product, the following powder formation rate 99.4% of 0.36mm.
Comparative Examples 4
With the 138g mass concentration be 21.8% sodium oleate join the dried glue of 460g N41 in, stir, stable after; With the 168ml volumetric concentration is that 25%NaCl solution and 262ml volumetric concentration are that 18% alum liquor joins in the knockouts, under the high-speed stirring condition of room temperature and 4000 rev/mins, above-mentioned latex is added in the flocculation agent; Keep constant temperature; And then to add 254g concentration be that 17.2% sodium fat synthesis is isolated, and accomplishes and isolate back intensification slaking, separates, dehydration.Drying makes powder N41 product, powder median size 1.5mm, powder formation rate 89%.
Embodiment 7
Get the NR latex of the dried glue of 460g, the adding mass concentration is 19.1% StNa 513g, mixes, and is cooled to-25 ℃, and the adding volumetric concentration is 24% CaCl
2Solution 82ml condenses, and last warp filters, washing is drying to obtain powder NR product, the following powder formation rate 99.4% of 0.38mm.
Claims (3)
1. the preparation method of a powdered rubber is characterized in that separant is joined in the rubber latex, fully mixes, and under agitation condition, adds the flocculation agent cohesion, and condensation temperature is-30～-5 ℃, makes powdered rubber through separation, dehydration, drying;
Described rubber latex is content of polybutadiene rubber latex, X 050 latex, styrene butadiene rubber latex, paracril latex, carboxy nitrile rubber latex, carboxylic styrene-butadiene rubber latex; Described separant is one or more in potassium stearate, StNa, potassium oleate, sodium oleate, synthetic fatty acid potassium, the sodium fat synthesis, and mass concentration is 16%～22%, weight by dry rubber, and per 100 mass parts latex add-ons are 0.1～20 part; Described flocculation agent is univalent metal salt, divalent metal salt or trivalent metal salt; Flocculation agent uses with aqueous solution form, and volumetric concentration is 2%～25%, weight by dry rubber, and per 100 mass parts latex add-ons are 0.1～25 part.
2. preparation method as claimed in claim 1 is characterized in that described condensation temperature is-15～-5 ℃.
3. preparation method as claimed in claim 1 is characterized in that described flocculation agent is selected from NaCl, KCl, CaCl
2, MgSO
4, in the alum one or more.
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| CN200910238563A CN102070789B (en) | 2009-11-25 | 2009-11-25 | Preparation method of powder rubber |
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|---|---|---|---|
| CN200910238563A CN102070789B (en) | 2009-11-25 | 2009-11-25 | Preparation method of powder rubber |
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| CN102070789A CN102070789A (en) | 2011-05-25 |
| CN102070789B true CN102070789B (en) | 2012-10-17 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 type separant |
| CN103204959B (en) * | 2012-01-16 | 2015-02-25 | 中国石油天然气股份有限公司 | Oil-extended powdery rubber preparation method |
| CN103804530B (en) * | 2012-11-14 | 2016-08-03 | 中国石油天然气股份有限公司 | A kind of preparation method of modified powder butadiene-styrene rubber |
| CN104761733A (en) * | 2015-03-29 | 2015-07-08 | 安徽同丰橡塑工业有限公司 | Preparation method of adhesive-type powder chloroprene rubber |
| US11161920B2 (en) * | 2017-03-28 | 2021-11-02 | Zeon Corporation | Method for producing carboxyl-group-containing nitrile rubber |
| CN108976446B (en) * | 2017-05-31 | 2021-04-13 | 中国石油化工股份有限公司 | Preparation method of powdered styrene butadiene rubber |
| CN109485753B (en) * | 2018-10-29 | 2019-12-03 | 青岛科技大学 | A kind of fresh latex flucculation process |
| WO2021003541A1 (en) * | 2019-07-11 | 2021-01-14 | LEMES, Jorge Antônio | Process of agglomeration by coacervation of vulcanized rubber powder and resulting product |
| CN111704772A (en) * | 2020-04-30 | 2020-09-25 | 浙江信汇新材料股份有限公司 | Granular butyl rubber composition with anti-sticking effect and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1704439A (en) * | 2004-06-02 | 2005-12-07 | 中国石油天然气股份有限公司 | Method for making powdered rubber |
| US7118494B2 (en) * | 2005-01-24 | 2006-10-10 | Bridgestone Sports Co., Ltd. | Multi-piece solid golf ball |
| CN1865306A (en) * | 2005-05-20 | 2006-11-22 | 中国石油天然气集团公司 | Low content nitrile cross-linked powdery acrylonitrile butadiene preparation method |
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2009
- 2009-11-25 CN CN200910238563A patent/CN102070789B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1704439A (en) * | 2004-06-02 | 2005-12-07 | 中国石油天然气股份有限公司 | Method for making powdered rubber |
| US7118494B2 (en) * | 2005-01-24 | 2006-10-10 | Bridgestone Sports Co., Ltd. | Multi-piece solid golf ball |
| CN1865306A (en) * | 2005-05-20 | 2006-11-22 | 中国石油天然气集团公司 | Low content nitrile cross-linked powdery acrylonitrile butadiene preparation method |
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