CN110564065A - Pre-dispersed master colloidal particle formula and preparation method thereof - Google Patents
Pre-dispersed master colloidal particle formula and preparation method thereof Download PDFInfo
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- CN110564065A CN110564065A CN201910877652.6A CN201910877652A CN110564065A CN 110564065 A CN110564065 A CN 110564065A CN 201910877652 A CN201910877652 A CN 201910877652A CN 110564065 A CN110564065 A CN 110564065A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2311/00—Characterised by the use of homopolymers or copolymers of chloroprene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/16—Ethene-propene or ethene-propene-diene copolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
- C08J2491/06—Waxes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/39—Thiocarbamic acids; Derivatives thereof, e.g. dithiocarbamates
- C08K5/405—Thioureas; Derivatives thereof
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Abstract
The invention relates to a formula of pre-dispersed master colloidal particles containing tetrahydro-2 (1H) -pyrithion and a preparation method of the formula. The formula comprises the following components in parts by weight: 73-77 parts of tetrahydro-2 (1H) -pyrimidine thione; 10-15 parts of a rubber carrier; 2-10 parts of an active agent component; 1-6 parts of hydrocarbon paraffin solid or fatty acid salt; 2-7 parts of paraffin oil. The preparation method comprises the following steps: firstly, preparing a rubber carrier; weighing the required raw materials; putting the raw materials into an internal mixer for internal mixing to obtain a sizing material; and finally, putting the rubber material into an extruder, controlling the given rotating speed of a main machine to be 115-125 r/min, and controlling the extrusion temperature to be 50-70 ℃ to prepare the pre-dispersed master batch containing the tetrahydro-2 (1H) -pyrimidinethione. The invention improves the dispersion problem of tetrahydro-2 (1H) -pyrimidinethione in rubber compounds, and simultaneously solves the problem of dust pollution caused by directly using tetrahydro-2 (1H) -pyrimidinethione. The pre-dispersed masterbatch particles have the characteristics of high vulcanization speed, high scorching safety, flat vulcanization, excellent thermal aging performance, no pollution, no coloring and no frost spraying for rubber, especially chloroprene rubber, can replace ETU (ethylene-butylene-terephthalate) which has reproductive toxicity and generates carcinogen nitrosamine in the vulcanization or use process, and has practical production value.
Description
Technical Field
the invention relates to the technical field of rubber additives and preparation thereof, in particular to a predispersed master batch particle formula containing tetrahydro-2 (1H) -pyrimidinethione and a preparation method of the formula.
Background
tetrahydro-2 (1H) -pyrimidine thione is one new kind of efficient green thiourea promoter, and as for halogenated polymer, tetrahydro-2 (1H) -pyrimidine thione as vulcanizing assistant can obtain high performance vulcanized rubber in short period and has high scorching stability. The tetrahydro-2 (1H) -pyrimidinethione is white powder, and can bring great benefits to rubber products, but in the processing process of the rubber products, the technical problems of roller sticking, dust flying, easy agglomeration, difficult dispersion and the like exist, and meanwhile, the health of staff is harmed and the metering is inaccurate. In actual operation, methods such as prolonging the mixing time and increasing the mixing temperature are often adopted to make up for the defects, and the methods affect the production efficiency, increase the energy consumption and increase the production cost.
The invention patent application with the application number of 201610703976.4 provides rubber accelerator N, N-ethylene thiourea pre-dispersed master batch and a preparation method thereof. However, when the N, N-ethylene thiourea is used as a rubber accelerator, a carcinogenic substance nitrosamine is generated in the vulcanization process, so that the environment is polluted and the health of operators is harmed.
Disclosure of Invention
the invention aims to provide pre-dispersed master batch particles which can realize rapid vulcanization and good scorching safety especially for chloroprene rubber so as to obtain high-performance vulcanized rubber and a preparation method thereof. In particular to a formula of pre-dispersed master colloidal particles containing tetrahydro-2 (1H) -pyrimidinethione and a preparation method of the formula.
The formula comprises the following components in parts by weight:
73-77 parts of tetrahydro-2 (1H) -pyrimidine thioketone
10-15 parts of rubber carrier
2-10 parts of active agent component
1-6 parts of hydrocarbon paraffin solid or fatty acid salt
2-7 parts of paraffin oil.
Further optimizing the formula of the pre-dispersed master batch, wherein the rubber carrier is composed of ethylene propylene diene monomer, ethylene propylene diene monomer and stearic acid, and the weight ratio of the ethylene propylene diene monomer to the stearic acid is 8-11: 1-5: 1.
The preparation method of the pre-dispersed masterbatch particle formula comprises the following steps:
Step 1, accurately weighing all raw materials required by the rubber carrier according to a ratio, firstly putting ethylene propylene diene monomer and ethylene propylene diene monomer into an internal mixer for mixing, then adding stearic acid for mixing, and preparing a sheet-shaped rubber carrier with the thickness of 2-20 mm on an open mill;
step 2, accurately weighing each raw material of the pre-dispersed masterbatch particle formula according to the proportion; putting the raw materials into an internal mixer, and mixing for 2-10 minutes at the temperature of 80-85 ℃ and the rotating speed of 55-60 rpm to obtain a rubber material;
And 3, putting the rubber material obtained in the step 2 into an extruder, controlling the given rotating speed of a main machine to be 115-125 r/min, and controlling the extrusion temperature to be 50-70 ℃ to obtain the pre-dispersed masterbatch particles containing the tetrahydro-2 (1H) -pyrimidinethione.
compared with the prior art, the pre-dispersed master colloidal particle formula and the preparation method thereof have the following beneficial effects:
(1) The tetrahydro-2 (1H) -pyrimidinethione is added into a rubber carrier according to a certain proportion, and a certain amount of active agent components, hydrocarbon paraffin wax solid or fatty acid salt and paraffin oil are added at the same time to prepare the tetrahydro-2 (1H) -pyrimidinethione-containing pre-dispersed master colloidal particle, wherein the pre-dispersed master colloidal particle improves the dispersion problem of tetrahydro-2 (1H) -pyrimidinethione powder in a rubber colloidal material while ensuring the activity of the tetrahydro-2 (1H) -pyrimidinetinethione, and simultaneously solves the problems of dust pollution, large metering error and roller sticking caused by directly using the tetrahydro-2 (1H) -pyrimidinethione.
(2) The pre-dispersed master batch has a simple formula and only comprises five components of tetrahydro-2 (1H) -pyrimidinethione, a rubber carrier, an active agent component, hydrocarbon paraffin solid or fatty acid salt and paraffin oil.
(3) The active ingredient tetrahydro-2 (1H) -pyrimidinethione in the pre-dispersed master colloidal particle formula has the advantages of high vulcanization speed, high scorch safety, flat vulcanization and excellent heat aging performance for rubber, especially chloroprene rubber.
(4) compared with the pre-dispersed masterbatch particle taking N, N-ethylene thiourea as an effective component, the pre-dispersed masterbatch particle does not generate carcinogenic substance nitrosamine in the vulcanization process, has the characteristics of no pollution, no coloring and no blooming, and is the first choice for replacing the N, N-ethylene thiourea.
Detailed Description
The invention discloses a formula of a pre-dispersed master colloidal particle containing tetrahydro-2 (1H) -pyrimidinethione and a preparation method of the formula, wherein the pre-dispersed master colloidal particle containing the tetrahydro-2 (1H) -pyrimidinethione is prepared by adding the tetrahydro-2 (1H) -pyrimidinethione into a rubber carrier according to a certain proportion and simultaneously adding a certain amount of active agent components, hydrocarbon paraffin wax solid or fatty acid salt and paraffin oil, and the pre-dispersed master colloidal particle ensures the activity of the tetrahydro-2 (1H) -pyrimidinethione, improves the dispersion problem of tetrahydro-2 (1H) -pyrimidinethione powder in a rubber colloidal material, and solves the problems of dust pollution, large metering error and roll sticking caused by directly using the tetrahydro-2 (1H) -pyrimidinethione.
The preparation method comprises the following steps:
Step 1, according to the weight ratio of 8-11 of ethylene propylene diene monomer, ethylene propylene diene monomer and stearic acid: 1-5: 1 accurately weighing all raw materials required by the rubber carrier, firstly putting ethylene propylene diene monomer and ethylene propylene diene monomer into an internal mixer for mixing, then adding stearic acid for mixing, and preparing the flaky rubber carrier with the thickness of 2-20 mm on an open mill.
step 2, accurately weighing all raw materials required by the rubber vulcanizing agent according to the proportion; and (3) putting the raw materials into an internal mixer, and mixing for 2-10 minutes at the temperature of 80-85 ℃ and the rotating speed of 55-60 rpm to obtain the rubber material.
And 3, putting the rubber material obtained in the step 2 into an extruder, controlling the given rotating speed of a main machine to be 115-125 r/min, and finally extruding to obtain the tetrahydro-2 (1H) -pyrimidinethione pre-dispersed master batch particles, wherein the extrusion temperature is 50-70 ℃.
The performance detection result of the prepared pre-dispersed master batch particle product is as follows:
Table one pre-dispersed masterbatch formulation for each example:
the preparation methods of the first embodiment, the second embodiment and the fifth embodiment are consistent, and the preparation method comprises the following steps:
Step 1, according to the weight ratio of ethylene propylene diene monomer, ethylene propylene diene monomer and stearic acid being 10: 3: 1 accurately weighing all raw materials required by the rubber carrier, firstly putting ethylene propylene diene monomer and ethylene propylene diene monomer into an internal mixer for mixing, then adding stearic acid for mixing, and preparing the flaky rubber carrier with the thickness of 3mm on an open mill.
step 2, accurately weighing all raw materials required by the rubber vulcanizing agent according to the proportion; putting the raw materials into an internal mixer, and mixing for 10min at the temperature of 80 ℃ and the rotating speed of 60rpm to obtain the rubber material.
and 3, putting the rubber material obtained in the step 2 into an extruder, controlling the given rotating speed of a main machine to be 120r/min, controlling the extrusion temperature to be 60 ℃, and extruding to obtain the dispersed masterbatch particles.
the preparation method of the third embodiment comprises the following steps:
step 1, according to the weight ratio of 8: 5: 1 accurately weighing all raw materials required by the rubber carrier, firstly putting ethylene propylene diene monomer and ethylene propylene diene monomer into an internal mixer for mixing, then adding stearic acid for mixing, and preparing the flaky rubber carrier with the thickness of 10mm on an open mill.
Step 2, accurately weighing all raw materials required by the rubber vulcanizing agent according to the proportion; the raw materials are put into an internal mixer and mixed for 2 minutes under the conditions of the temperature of 80 ℃ and the rotating speed of 55rpm to obtain the rubber material.
And 3, putting the rubber material obtained in the step 2 into an extruder, controlling the given rotating speed of a main machine to be 115r/min, controlling the extrusion temperature to be 50 ℃, and extruding to obtain the pre-dispersed masterbatch particles.
The preparation method of the embodiment IV comprises the following steps:
Step 1, according to the weight ratio of ethylene propylene diene monomer, ethylene propylene diene monomer and stearic acid being 11: 1: 1 accurately weighing each raw material required by the rubber carrier, firstly putting ethylene propylene diene monomer and ethylene propylene diene monomer into an internal mixer for mixing, then adding stearic acid for mixing, and preparing the mixture into a sheet with the thickness of 20mm on an open mill.
Step 2, accurately weighing all raw materials required by the rubber vulcanizing agent according to the proportion; the raw materials are put into an internal mixer and mixed for 10 minutes under the conditions of 85 ℃ and 60rpm of rotating speed, and the rubber material is obtained.
And 3, putting the rubber material obtained in the step 2 into an extruder, controlling the given rotating speed of a main machine to be 125r/min, controlling the extrusion temperature to be 70 ℃, and extruding to obtain the pre-dispersed masterbatch particles.
The two pre-dispersed masterbatch particles of the first embodiment and the second embodiment are respectively used as accelerators to be applied to chloroprene rubber, wherein the raw materials are proportioned (in parts by mass): 100 parts of chloroprene rubber, 4 parts of zinc oxide, 5 parts of aromatic oil, 50 parts of N550 carbon black, 40101 parts of anti-aging agent, HT 2222 parts of lubricant and 0.5 part of accelerator.
Chloroprene rubber, N550 carbon black, aromatic oil, an anti-aging agent 4010 and a lubricant are mixed in an internal mixer to prepare chloroprene rubber compound. Adding zinc oxide, an accelerant and tapping rubber on an open mill at the temperature of 40 ℃ for 3 times, uniformly mixing, thinly passing and packaging by a triangular bag for 6 times, adjusting the roller spacing to 2mm, and discharging. After standing at room temperature for 16h, vulcanized samples were prepared on a press vulcanizer to obtain the application sample of example one and the application sample of example two.
the vulcanization behaviour of the mixes was tested in accordance with GB/T16584-1996, the results of which are shown in Table II.
Vulcanization characteristics of the surfacer rubber
As can be seen from Table II, the product of example I has good scorch safety, fast vulcanization speed and high crosslinking degree during the vulcanization of chloroprene rubber.
Testing the vulcanized sample, wherein the tensile property is tested according to GB/T528-2009; the Shore A hardness is tested according to GB/T531.1-2008; the hot air aging performance is tested according to GB/T3512-2014, the temperature is 100 ℃, the aging time is 48h, and the test results are shown in Table three and Table four.
physical and mechanical properties of watch trisulfide sample
EXAMPLES one application sample and two application samples of example were aged at 100 ℃ for 48 hours, and the properties of the vulcanized samples are shown in Table four.
Physical and mechanical properties of aged vulcanized rubber at 100 ℃ for 48h in Table IV
As can be seen from the table III and the table IV, the product of the example I is used as an accelerator to vulcanize chloroprene rubber, the physical and mechanical properties of the vulcanized rubber obtained are not much different from those of the chloroprene rubber disulfide of the example, but the retention rates of tensile strength and elongation at break after aging are higher, which indicates that the thermal aging performance is better.
the invention is described above by way of example, and it is obvious that the implementation of the invention is not limited by the above-described manner, and it is within the scope of the invention to apply the inventive concept and solution to other applications without modification, or to apply the inventive concept and solution to other applications directly.
Claims (3)
1. A pre-dispersed master colloidal particle formula is characterized in that: the pre-dispersion master colloidal particle formula comprises the following components in parts by weight:
73-77 parts of tetrahydro-2 (1H) -pyrimidine thioketone
10-15 parts of rubber carrier
2-10 parts of active agent component
1-6 parts of hydrocarbon paraffin solid or fatty acid salt
2-7 parts of paraffin oil.
2. the pre-dispersed masterbatch particle formulation of claim 1, wherein: the rubber carrier is composed of ethylene propylene diene monomer, ethylene propylene diene monomer and stearic acid, wherein the mass ratio of the ethylene propylene diene monomer to the stearic acid is 8-11: 1-5: 1.
3. A method of preparing a pre-dispersed masterbatch pellet formulation according to claim 1, wherein said method comprises the steps of: the method comprises the following steps:
Step 1, weighing raw materials of the rubber carrier according to a ratio, firstly putting ethylene propylene diene monomer and ethylene propylene diene monomer into an internal mixer for mixing, then adding stearic acid for mixing, and after rubber discharge, preparing the rubber carrier with a sheet shape on an open mill;
Step 2, weighing the raw materials of the pre-dispersed masterbatch particle formula according to the proportion; putting the raw materials into an internal mixer, and mixing for 2-10 minutes at the temperature of 80-85 ℃ and the rotating speed of 55-60 rpm to obtain a rubber material;
And 3, putting the rubber material obtained in the step 2 into an extruder, controlling the given rotating speed of a main machine to be 115-125 r/min, and controlling the extrusion temperature to be 50-70 ℃ to obtain the pre-dispersed masterbatch particles containing the tetrahydro-2 (1H) -pyrimidinethione.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2544746A (en) * | 1949-07-27 | 1951-03-13 | Du Pont | Vulcanization of chloroprene polymers |
| CN106188819A (en) * | 2016-08-23 | 2016-12-07 | 宁波硫华聚合物有限公司 | Pre-dispersed masterbatch particles of rubber accelerator ETU and preparation method thereof |
| CN108864579A (en) * | 2018-07-11 | 2018-11-23 | 宁波艾克姆新材料有限公司 | Pre-dispersed masterbatch particles of diphenylguanidine and preparation method thereof |
| CN109181044A (en) * | 2018-07-11 | 2019-01-11 | 宁波艾克姆新材料有限公司 | Pre-dispersed masterbatch particles of rubber antioxidant ZMMBI and preparation method thereof |
-
2019
- 2019-09-17 CN CN201910877652.6A patent/CN110564065A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2544746A (en) * | 1949-07-27 | 1951-03-13 | Du Pont | Vulcanization of chloroprene polymers |
| CN106188819A (en) * | 2016-08-23 | 2016-12-07 | 宁波硫华聚合物有限公司 | Pre-dispersed masterbatch particles of rubber accelerator ETU and preparation method thereof |
| CN108864579A (en) * | 2018-07-11 | 2018-11-23 | 宁波艾克姆新材料有限公司 | Pre-dispersed masterbatch particles of diphenylguanidine and preparation method thereof |
| CN109181044A (en) * | 2018-07-11 | 2019-01-11 | 宁波艾克姆新材料有限公司 | Pre-dispersed masterbatch particles of rubber antioxidant ZMMBI and preparation method thereof |
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