CN105670066A - Rubber accelerator, activator and magnesium oxide masterbatches and preparation method therefor - Google Patents
Rubber accelerator, activator and magnesium oxide masterbatches and preparation method therefor Download PDFInfo
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- CN105670066A CN105670066A CN201610261627.1A CN201610261627A CN105670066A CN 105670066 A CN105670066 A CN 105670066A CN 201610261627 A CN201610261627 A CN 201610261627A CN 105670066 A CN105670066 A CN 105670066A
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- magnesium oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
-
- 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
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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
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a preparation method for rubber accelerator, activator and magnesium oxide masterbatches. The method comprises the steps of in parts by weight, stirring and mixing 35-60 parts of a magnesium chloride solution with the mass concentration of 45%, 5-10 parts of triethylhexyl phosphonic acid and 35-55 parts of a sodium carbonate solution with the mass concentration of 50%; stirring a mixture in a constant-temperature water bath with the temperature of 60-80 DEG C at a speed of 600-800r/min until no sediments are generated; and slowly reducing the stirring speed for static settlement.
Description
Technical field
The present invention relates to chemical field, specifically, the present invention relates to rubber accelerator activating agent magnesium oxide masterbatch particles and preparation method thereof.
Background technology
Pre-dispersed masterbatch particles is a kind of physical mixture being configured to carrier by one matter or some materials. The pre-dispersed masterbatch particles making this change application form or change form is intended to optimize material to be suitable for its special application scenario. In rubber industry, the demand of pre-dispersed masterbatch particles is increased day by day, and various forms of kind is developed in succession. Pre-dispersed masterbatch particles, except improving wholesomeness and safety, also has the superiority of economic aspect.
Powder body in pre-dispersed masterbatch particles refers generally to sulfur, various accelerator etc. Except indexs such as conventional density, ash, outward appearances, in addition it is also necessary to detection sulfur content, oil factor, screening thing, to the raw material often having Mooney to fluctuate, it is necessary to control particle size distribution. Generally, specific surface area is more high, and mean diameter is more little, and oil factor is more high, then the Mooney point of the product of production is more high. So not more thin more good when selecting raw material, more thin raw material can bring processing difficulties, disperses the problems such as bad, but simultaneously, selected thick raw material, and that just loses pre-dispersed meaning.
Summary of the invention
It is an object of the invention to provide rubber accelerator activating agent magnesium oxide masterbatch particles and preparation method thereof.
In order to realize the purpose of the present invention, the preparation method that the present invention provides rubber accelerator activating agent magnesium oxide masterbatch particles, the method includes: (1) counts by weight, choose the magnesium chloride solution that mass concentration is 45% of 35～60 parts, the triethyl group hexyl phosphoric acid of 5～10 parts, the mass concentration of 35～55 parts is the sodium carbonate liquor of 50%, it is stirred for mixing and is placed in 60～80 DEG C of waters bath with thermostatic control, under 600～800r/min, stirring produces to without precipitation, slowly reduce mixing speed subsequently so that it is staticly settle 20～30min;
(2) after staticly settling, to its vacuum filtration, and be 7.0 with deionized water washing sediment to pH, being subsequently placed at temperature is after drying 2～3 hours at 95～100 DEG C, take out, and after the 10～15min that mills under 5～10MPa, be placed in crucible, at 200～300 DEG C, calcine 2～3h, be prepared into the calcined oxide magnesium dust of 100～120 orders;
(3) above-mentioned prepared magnesium oxide powder is placed in point-like 60Co radiation side and carries out pre-irradiated 10～15min, 1:3:5 in mass ratio subsequently, stir to be mixed to form with deionized water and styrene by the magnesium oxide powder after pre-irradiated and mix turbid liquid, by the copper-bath mass ratio 1:1 that the magnesium oxide powder after pre-irradiated and mass concentration are 20%, the copper-bath that mass concentration is 20% is placed in the turbid liquid of above-mentioned mixing, stirs mixing 10～15min;
(4) after its stirring mixing completes, it is placed in irradiation devices so that it is be warming up to 45～50 DEG C, after it is carried out evacuation, passing into argon again, be placed in gamma-ray irradiation source chamber by the airtight irradiation devices of above-mentioned full argon and carry out irradiation, exposure time is 20～30min;
(5) to be irradiated complete after, by the magnesium oxide powder of graft phenylethene, by liquid benzene extracting 10～12h, will be drawn off subsequently, be placed in the baking oven of 80～90 DEG C dry 3～5h, prepare styrene-grafted magnesium oxide powder;
(6) count by weight, choose the styrene-grafted magnesium oxide powder stirring mixing of the butadiene-styrene rubber granule of 75～95 parts, the epoxy soybean oil of 1～5 part, the liquid paraffin of 2～10 parts and 2～10 parts, it is placed in double screw extruder, extruding pelletization at 150～170 DEG C, to obtain final product.
Preferably, the step (1) of the method is additionally added sulfamic acid { (1S, 2S, 4R)-4-[(5-{ [1-(3-Brombenzyl)-1H-pyrazole-3-yl] carbonyl } pyrimidine-4-yl) amino]-2-hydroxycyclopent base } methyl ester.
The present invention also provides for sulfamic acid { (1S, 2S, 4R)-4-[(5-{ [1-(3-Brombenzyl)-1H-pyrazole-3-yl] carbonyl } pyrimidine-4-yl) amino]-2-hydroxycyclopent base } methyl ester is as the purposes in antibacterial.
The invention has the beneficial effects as follows:
(1) the pre-dispersed masterbatch particles good product dispersibility of modified oxidized magnesium, be beneficial in mixing process absorb and ensure effective ingredient optimum activity, reduce mixing time;
(2) good fluidity, without dust from flying, will not lump under normal storage conditions;
(3) operating procedure is simple, and cost is low.
Detailed description of the invention
Below by way of the description of detailed description of the invention, the invention will be further described, but this is not limitation of the present invention, those skilled in the art's basic thought according to the present invention, various modifications may be made or improves, but without departing from the basic thought of the present invention, all within the scope of the present invention.
Embodiment 1
Use sulfamic acid { (1S, 2S, 4R)-4-[(5-{ [1-(3-Brombenzyl)-1H-pyrazole-3-yl] carbonyl } pyrimidine-4-yl) amino]-2-hydroxycyclopent base } methyl ester, filter paper enzyme classical in this area is adopted to carry out bacteriostatic test, for examination strain fermentation cellulomonas cartae ATCC43279 purchased from Fu Xiang bio tech ltd, Shanghai.
Culture fluid
Nutrient agar and nutrient broth, purchased from Chen Yu experimental facilities company limited of BeiJing ZhongKe.
Test method
Fermentable fiber Zymomonas mobilis ATCC43279 is inoculated in agar plate nutritional solution plane, uniformly gathers during inoculation.
Weighing target compound 0.01 gram, add 15000 ml sterile waters, ultrasonic 30 minutes, then the filtering with microporous membrane of 0.22 μm, obtained solution. The aseptic circular filter paper sheet of tweezer, sprays above-mentioned solution to complete wetting, is attached in the agar plate nutritional solution plane of inoculated bacteria. Agar plate is placed in the incubator of 37 DEG C, incubation 4 hours. Measure the diameter of antibacterial ring. Measure and average for 3 times.
1.4 results
The average diameter of the antibacterial ring of fermentable fiber Zymomonas mobilis ATCC43279 is 12.26mm, and this shows that target compound has the effect of extremely strong vitro inhibition fermentable fiber Zymomonas mobilis ATCC43279.
Claims (3)
1. the preparation method of rubber accelerator activating agent magnesium oxide masterbatch particles, the method includes: (1) counts by weight, choose the magnesium chloride solution that mass concentration is 45% of 35～60 parts, the triethyl group hexyl phosphoric acid of 5～10 parts, the mass concentration of 35～55 parts is the sodium carbonate liquor of 50%, is stirred for mixing and is placed in 60～80 DEG C of waters bath with thermostatic control, and under 600～800r/min, stirring produces to without precipitation, slowly reduce mixing speed subsequently so that it is staticly settle 20～30min;
(2) after staticly settling, to its vacuum filtration, and be 7.0 with deionized water washing sediment to pH, being subsequently placed at temperature is after drying 2～3 hours at 95～100 DEG C, take out, and after the 10～15min that mills under 5～10MPa, be placed in crucible, at 200～300 DEG C, calcine 2～3h, be prepared into the calcined oxide magnesium dust of 100～120 orders;
(3) above-mentioned prepared magnesium oxide powder is placed in point-like 60Co radiation side and carries out pre-irradiated 10～15min, 1:3:5 in mass ratio subsequently, stir to be mixed to form with deionized water and styrene by the magnesium oxide powder after pre-irradiated and mix turbid liquid, by the copper-bath mass ratio 1:1 that the magnesium oxide powder after pre-irradiated and mass concentration are 20%, the copper-bath that mass concentration is 20% is placed in the turbid liquid of above-mentioned mixing, stirs mixing 10～15min;
(4) after its stirring mixing completes, it is placed in irradiation devices so that it is be warming up to 45～50 DEG C, after it is carried out evacuation, passing into argon again, be placed in gamma-ray irradiation source chamber by the airtight irradiation devices of above-mentioned full argon and carry out irradiation, exposure time is 20～30min;
(5) to be irradiated complete after, by the magnesium oxide powder of graft phenylethene, by liquid benzene extracting 10～12h, will be drawn off subsequently, be placed in the baking oven of 80～90 DEG C dry 3～5h, prepare styrene-grafted magnesium oxide powder;
(6) count by weight, choose the styrene-grafted magnesium oxide powder stirring mixing of the butadiene-styrene rubber granule of 75～95 parts, the epoxy soybean oil of 1～5 part, the liquid paraffin of 2～10 parts and 2～10 parts, it is placed in double screw extruder, extruding pelletization at 150～170 DEG C, to obtain final product.
2. method according to claim 1, it is characterized in that, the step (1) of the method is additionally added sulfamic acid { (1S, 2S, 4R)-4-[(5-{ [1-(3-Brombenzyl)-1H-pyrazole-3-yl] carbonyl } pyrimidine-4-yl) amino]-2-hydroxycyclopent base } methyl ester.
3. sulfamic acid { (1S, 2S, 4R)-4-[(5-{ [1-(3-Brombenzyl)-1H-pyrazole-3-yl] carbonyl } pyrimidine-4-yl) amino]-2-hydroxycyclopent base } methyl ester is as the purposes in antibacterial.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610261627.1A CN105670066A (en) | 2016-04-22 | 2016-04-22 | Rubber accelerator, activator and magnesium oxide masterbatches and preparation method therefor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610261627.1A CN105670066A (en) | 2016-04-22 | 2016-04-22 | Rubber accelerator, activator and magnesium oxide masterbatches and preparation method therefor |
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| CN105670066A true CN105670066A (en) | 2016-06-15 |
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| CN201610261627.1A Pending CN105670066A (en) | 2016-04-22 | 2016-04-22 | Rubber accelerator, activator and magnesium oxide masterbatches and preparation method therefor |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079533A (en) * | 2010-12-03 | 2011-06-01 | 桐柏兴源化工有限公司 | Method for preparing basic magnesium carbonate and high purity magnesium oxide with trona |
| CN102924829A (en) * | 2012-11-08 | 2013-02-13 | 沈阳化工大学 | Zinc oxide pre-dispersion master colloidal particle and preparation method thereof |
| CN105419022A (en) * | 2015-12-03 | 2016-03-23 | 雷春生 | Preparation method of modified magnesium oxide pre-dispersed rubber masterbatch |
| CN105492429A (en) * | 2013-07-02 | 2016-04-13 | 米伦纽姆医药公司 | Heteroaryl inhibitors of SUMO activating enzyme |
-
2016
- 2016-04-22 CN CN201610261627.1A patent/CN105670066A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079533A (en) * | 2010-12-03 | 2011-06-01 | 桐柏兴源化工有限公司 | Method for preparing basic magnesium carbonate and high purity magnesium oxide with trona |
| CN102924829A (en) * | 2012-11-08 | 2013-02-13 | 沈阳化工大学 | Zinc oxide pre-dispersion master colloidal particle and preparation method thereof |
| CN105492429A (en) * | 2013-07-02 | 2016-04-13 | 米伦纽姆医药公司 | Heteroaryl inhibitors of SUMO activating enzyme |
| CN105419022A (en) * | 2015-12-03 | 2016-03-23 | 雷春生 | Preparation method of modified magnesium oxide pre-dispersed rubber masterbatch |
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Address after: 315033 Zhejiang Province, Ningbo Jiangbei District Haichuan Road 168 Lane No. 1 Applicant after: Ningbo acme New Material Co. Ltd. Address before: 315033 Zhejiang Province, Ningbo Jiangbei District Hongtang street small Lang Industrial Zone Applicant before: Ningbo Actmix Polymer Co., Ltd. |
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Application publication date: 20160615 |
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