CN1031716C - Preparation method of nitrile-butadiene rubber powder - Google Patents
Preparation method of nitrile-butadiene rubber powder Download PDFInfo
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- CN1031716C CN1031716C CN 93101142 CN93101142A CN1031716C CN 1031716 C CN1031716 C CN 1031716C CN 93101142 CN93101142 CN 93101142 CN 93101142 A CN93101142 A CN 93101142A CN 1031716 C CN1031716 C CN 1031716C
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- butadiene rubber
- nitrile
- rubber powder
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- rubber
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Abstract
The present invention relates to a preparation method of nitrile-butadiene rubber powder. A water solution of univalent metal salts and a water solution of divalent metal salts are added into nitrile-butadiene rubber latex in segments, a separating agent is automatically generated in the system through precoagulation, flocculation, rubber particle hardening and rubber particle spheroidization, and the purpose of active isolation can be achieved. Rubber particles after being filtered, washed, dehydrated and dried are ground and sieved by a corresponding device to obtain the nitrile-butadiene rubber powder with the suitable particle diameter. The nitrile-butadiene rubber powder can be compatible with various resins so that a resin product has favorable water resistance, oil resistance, toughness, abrasion resistance, etc. The nitrile-butadiene rubber powder is widely suitable for the serialization and the automatization of the processing procedures of rubber modified polyvinyl chloride, etc. The present invention has the advantages of simple preparation technology, easy device fabrication, high latex content of the product and obvious economic benefit.
Description
The method that the present invention is a kind of segmentation cohesion, activity is isolated, wet grinding prepares acrylonitrile-butadiene rubber powder, it is the new technology in China Synthetic Rubber Industry field.
Acrylonitrile-butadiene rubber powder and various kinds of resin blend have good consistency, therefore are mainly used in resin modified.In polyvinyl chloride, add elasticity, water tolerance and the oil-proofness that a small amount of acrylonitrile-butadiene rubber powder can improve goods; Also can greatly 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; Acrylonitrile-butadiene rubber powder and resol and usefulness have plastification or the like.
Acrylonitrile-butadiene rubber powder is compared with block paracril, 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.
At present, the preparation acrylonitrile-butadiene rubber powder, the main method that adopts has: mechanical crushing method, spray-drying process, expansion drying method, starch-xanthation compound coagulation method, the carbon black precipitator method and dried emulsion method etc.Shortcomings such as suchlike method exists all that energy consumption height, granularity are big, poor water resistance and foreign matter content height.
It is different to the object of the present invention is to provide a kind of and existing coacervation to prepare acrylonitrile-butadiene rubber powder, and is furnished with the segmentation cohesion of relevant device, active isolated method.
Coacervation of the present invention prepares acrylonitrile-butadiene rubber powder, adopt the method for segmentation spraying cohesion, with the aqueous solution of monovalence and divalent metal salt be flocculation agent promptly: nitrile rubber is at the soft salt solution, under the effect of three kinds of flocculation agent of high rigidity salt solution and Adlerika (or calcium chloride solution), make latex pre-coagulate, flocculation, micelle nodularization, active isolate and process such as aftertreatment in make acrylonitrile-butadiene rubber powder.
Preparation process of the present invention is: the special-purpose nitrile rubber that will prepare promptly gets acrylonitrile-butadiene rubber powder through condensation powdering, antiseized isolation processing, filtration, dehydration, drying and process such as sieve.
For achieving the above object, now be described in detail the technological process of segmentation cohesion preparation acrylonitrile-butadiene rubber powder of the present invention.
1. latex preparation: with feed intake 6% potassium stearate and potassium oleate of amount of monomer of polymerization is emulsifying agent, under 40～60 ℃ temperature, carry out letex polymerization, when transformation efficiency is 95% when above, just make cross-linking type butyronitrile latex:, just make high temperature non-crosslinked type nitrile rubber when transformation efficiency is 75% when following.
When if emulsifying agent is selected synthetic fatty acid potassium and potassium oleate for use, its consumption is that polymerization 3% of the amount of monomer that feeds intake is carried out letex polymerization under 5～8 ℃ temperature, and its transformation efficiency is 75% o'clock, can make low temperature non-crosslinked type nitrile rubber.
More than prepared cross-linking type and non-crosslinked type nitrile rubber, the requirement of root a tree name product grade all can be used as the raw material of agglomeration process.
2. segmentation cohesion: with soft salt solution, high rigidity salt solution and three kinds of flocculation agent of Adlerika (or calcium chloride solution), in still formula equipment, divide three sections sprayings to add, its proportioning is: dried glue: salt: sal epsom (or calcium chloride)=1: 0.3～0.7: 0.02～0.08, condensation temperature are 30～65 ℃.
Under violent stirring, at first spraying adds soft, concentration is the salt solution of 25% (weight), is the pre-process of coagulating; Again with the high rigidity salt solution of concentration 25% (weight), under continuing to stir, add, and control spraying adding speed is carried out second section cohesion and is flocculation process; At last stirring velocity being improved, is that the Adlerika (or calcium chloride solution) of 8～10% (weight) carries out the 3rd section spraying cohesion with concentration, is the micelle nodularization process of hardening.As behind the powder, add the potassium stearate solution (or Magnesium Stearate or silicon sol) of 0～6% (weight) of dried glue amount again, as a supplement separant.Operation steps by segmentation cohesion of the present invention can reduce cohesion speed, but makes all condensation powderings of multiple latex.
3. active isolation the: in condensed system, the emulsifying agent potassium stearate, perhaps synthetic fatty acid potassium and potassium oleate, all can generate Magnesium Stearate (calcium) with the magnesium calcium ion in salt solution and sal epsom (or calcium chloride) solution, magnesium oleate (calcium), perhaps synthetic fatty acid magnesium (calcium) precipitates, and is in molecularity.When temperature was 50～65 ℃, the micelle that cohesion forms was very strong to its adsorption activity, therefore just produced active buffer action, obtained spontaneous separant.
If with cross-linking type or high temperature non-crosslinked type nitrile rubber is raw material, Cheng Fenhou can no longer add separant; If with low temperature non-crosslinked nitrile rubber is raw material,, and there is not potassium stearate because emulsification dosage is less, so as behind the powder, add the potassium stearate solution (or Magnesium Stearate or silicon sol) of 4～6% (in dried glue weight), separant all can reach active isolated purpose as a supplement.
4. grind and sieve:, in the adding material-twisting machine grinding is sieved and carry out simultaneously the filter cake of the nitrile rubber powder after centrifuge washing, the dehydration.Be the requirement that is suitable for grinding, be pressed on the filter cake at the rubber claw of adorning a rotation on the shredder, and contact grinding with screen cloth.Sieve through grinding, separant and micelle adhere to tightlyer, and the particle of pulverizing adheres to separant again, better effects if, and particle is thinner.Its particle diameter reaches below the 0.45mm.Adopt the corresponding sieve apparatus that ground of the present invention that powder formation rate is reached more than 95%.
The method that the present invention prepares acrylonitrile-butadiene rubber powder has the following advantages: (1) Production Flow Chart is short, and technology is simple, grinds sieve apparatus and easily makes; (2) the segmentation condensing method has spontaneous buffer action in agglomeration process, and isolation effect is good, the powder formation rate height; (3) particle diameter that adopts the present invention to prepare acrylonitrile-butadiene rubber powder suits, and is widely used, and has tangible economic benefit.
Embodiment 1
In 75 liters collection surface, add 10 kilograms of cross-linking types (or high temperature non-crosslinked type) nitrile rubber, under agitation spray into the soft salt solution that 3 liters of concentration are 25% (weight), spray into the high rigidity salt solution that 3 liters of concentration are 25% (weight) again, spraying into 2 liters of concentration again is the hard and infertile acid magnesium solution of 8% (weight), is warming up to 50 ℃, the discharging of lowering the temperature then, filter, washing, grinding is sieved, and is drying to obtain qualified product.
Embodiment 2
In 75 liters collection surface, add 10 kilograms of low temperature non-crosslinked type nitrile rubberes, under agitation spray into the soft salt solution that 3 liters of concentration are 25% (weight), spray into the high rigidity salt solution that 3 liters of concentration are 25% (weight) again, the Adlerika that to spray into 2 liters of concentration again be 8% (weight) adds the potassium stearate solution of 5% (in dry glue powder weight), be warming up to 55 ℃, the discharging of lowering the temperature is then filtered, washing, grinding is sieved, and is drying to obtain qualified product.
Embodiment 3
In 75 liters collection surface, add 10 kilograms of low temperature non-crosslinked type nitrile rubberes, under agitation spray into the soft salt solution that 3 liters of concentration are 25% (weight), spray into the high rigidity salt solution that 2 liters of concentration are 25% (weight) again, the calcium chloride solution that to spray into 2 liters of concentration again be 10% (weight) adds the Magnesium Stearate of 5% (in dry glue powder weight), be warming up to 60 ℃, the discharging of lowering the temperature is then filtered, washing, grinding is sieved, and is drying to obtain qualified product.
Embodiment 4
In 75 liters collection surface, add 10 kilograms of low temperature non-crosslinked type nitrile rubberes, under agitation spray into the soft salt solution that 3 liters of concentration are 25% (weight), spray into the high rigidity salt solution that 3 liters of concentration are 25% (weight) again, the Adlerika that to spray into 1.5 liters of concentration again be 8% (weight), the silicon sol that adds 6% (in dried glue weight), be warming up to 65 ℃, the discharging of lowering the temperature then, cohesion, filter, washing, grinding is sieved, and is drying to obtain qualified product.
Claims (3)
1. method for preparing acrylonitrile-butadiene rubber powder with segmentation cohesion, it is characterized in that in the nitrile rubber of preparation, dividing three sections sprayings to add soft salt solution, high rigidity salt solution and sal epsom (or calcium chloride) solution and make flocculation agent, its proportioning is: dried glue: salt: sal epsom (or calcium chloride)=1: 0.3～0.7: 0.02～0.08, coagulate in advance under 30～65 ℃ of temperature, flocculation is condensed into micelle, nodularization, the active isolation, wet grinding is sieved, and makes acrylonitrile-butadiene rubber powder at last.
2. the method for preparing acrylonitrile-butadiene rubber powder according to claim 1, it is characterized in that preparing emulsifying agent potassium stearate that nitrile rubber adds, potassium oleate, synthetic fatty acid potassium under 50～65 ℃ of temperature with flocculation agent in the magnesium calcium ion generate active separant, when its raw material was cross-linking type or high temperature non-crosslinked type nitrile rubber, Cheng Fenhou can not add separant; When its raw material was low temperature non-crosslinked type nitrile rubber, Cheng Fenhou added the separant of 4～6% (in the dry glue powder weight), reaches active isolation effect.
3. the method for preparing rubber powder according to claim 1, the wet grinding process of sieving that it is characterized in that the paracril grain behind the condensation powdering be in the grinding that the rubber claw is arranged grind simultaneously on the sieve apparatus and sieve, make the following fine powder of 0.45mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93101142 CN1031716C (en) | 1993-01-19 | 1993-01-19 | Preparation method of nitrile-butadiene rubber powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93101142 CN1031716C (en) | 1993-01-19 | 1993-01-19 | Preparation method of nitrile-butadiene rubber powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1083827A CN1083827A (en) | 1994-03-16 |
| CN1031716C true CN1031716C (en) | 1996-05-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93101142 Expired - Lifetime CN1031716C (en) | 1993-01-19 | 1993-01-19 | Preparation method of nitrile-butadiene rubber powder |
Country Status (1)
| Country | Link |
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| CN (1) | CN1031716C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007024008A1 (en) * | 2007-05-22 | 2008-11-27 | Lanxess Deutschland Gmbh | nitrile rubbers |
| CN101925614B (en) * | 2008-01-29 | 2013-08-07 | 朗盛德国有限责任公司 | Nitrile rubbers which optionally contain alkylthio terminal groups and which are optionally hydrogenated |
| CN103113597B (en) * | 2013-01-30 | 2018-07-27 | 怡维怡橡胶研究院有限公司 | Rubber masterbatch prepared by the method for continuously producing and this method of rubber masterbatch |
-
1993
- 1993-01-19 CN CN 93101142 patent/CN1031716C/en not_active Expired - Lifetime
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| Publication number | Publication date |
|---|---|
| CN1083827A (en) | 1994-03-16 |
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| C14 | Grant of patent or utility model | ||
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Free format text: CORRECT: PATENTEE; FROM: CHINA PETRO-CHEMICAL CORP.; CHINA PETROCHEMICAL, LANZHOU CHEMICAL INDUSTRYCO., LTD. TO: CHINA PETROCHEMICAL CORPORATION; LANZHOU CHEMICAL INDUSTRY CO., LTD., CHINA PETROCHEMICAL CORP. |
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| CP01 | Change in the name or title of a patent holder |
Patentee after: China Petrochemical Group Corp. Patentee after: Lanzhou Chemical Industry Co.,China National Petroleum Corp. Patentee before: China Petrochemical Corporation Patentee before: Lanzhou Chemical Industry Co., China Petrochemical Corp. |
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Expiration termination date: 20130119 Granted publication date: 19960501 |