CN103351477A - Modified microsphere master batch of foaming agent and preparation method for modified microsphere master batch of foaming agent - Google Patents
Modified microsphere master batch of foaming agent and preparation method for modified microsphere master batch of foaming agent Download PDFInfo
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Abstract
The invention provides a modified microsphere master batch of a foaming agent, which comprises the following components in parts by weight: 40-300 parts of foaming agent, 100 parts of an organic vehicle material and 2-4 parts of a dispersing agent. The invention further provides a preparation method for the modified microsphere master batch of the foaming agent. The modified AC microsphere master batch of the foaming agent adopts the surface treatment technology to realize the master batch of the foaming agent, has high dispersibility and consistency with organic polymer materials, is uniform in foaming, safe and convenient to use and store, greatly reduces potential production safety hazards and environmental harm in production, and improves safety of the foaming agent in transportation, storage and use.
Description
Technical Field
The invention relates to the field of foaming agent application, in particular to a composition of a modified foaming agent microbead master batch used in PP, PE, PVC, PET and plastic-wood products and a preparation method thereof.
Background
The chemical name of the AC foaming agent is azodicarbonamide (H)2NCON), AC foaming agents are prepared by oxidation of diurea as a yellowish or orange crystalline powder. Its molecular weight is 116, the decomposition heat is 359.9J/g deg.C, and the gases released by decomposition are mainly nitrogen (65%), carbon monoxide (32%) and a small amount of carbon dioxide (3%). The decomposed solid residues are mainly biurea, cyanuric acid and urazole. Slightly ammoniacal smell, nonflammable and self-extinguishing property when decomposed.
The AC foaming agent is widely used in the processing processes of polyvinyl chloride, polyethylene, polystyrene, ethylene-vinyl acetate copolymer, ABS resin, various rubbers and the like, has the characteristics of large foaming amount, short decomposition time, no combustion supporting, no toxicity, no odor, no pollution, fine particles, easy decomposition and use under normal pressure and pressurization, and is widely applied at home and abroad.
As an excellent foaming agent, a foaming agent which can replace AC has not been provided, but the pure AC foaming agent has certain defects which are mainly reflected in the influence of decomposition temperature, decomposition speed, decomposition products and the like on products. In order to improve the deficiencies of the foaming agent, the AC foaming agent is modified and improved from 20 century 70 years abroad, and a large number of patents are applied. Meanwhile, many new varieties are marketed.
The modification of the foaming agent AC product is to optimize the gas forming amount, granularity and thermal decomposition temperature of the foaming agent by changing certain reaction conditions or adding certain auxiliary agents in the preparation process, particularly in the oxidation process. The modified AC foaming agent mainly has the following aspects:
1) the grain size is ultra-fine. The common AC foaming agent has coarse average grain diameter and wide distribution, can not meet the production requirement of small and compact bubble pore diameter as required by artificial leather, and can be produced when the grain diameter d95 of the ultra-fine grain diameter type AC foaming agent is less than or equal to 8. The AC foaming agent produced under the condition of the prior art (such as urea method) can obtain different grades of ultra-fine AC foaming agents defined according to different particle diameters by crushing and grading so as to adapt to the foaming requirements of different plastic and rubber products.
2) A decomposition temperature lowering type. The low-temperature type AC foaming agent is decomposed at the temperature of 135-195 ℃, is adaptive to the softening temperature and the crosslinking temperature of resin and rubber, and is suitable for some resins and rubbers with low softening points and easy aging under heat. In the technological process of oxidizing biurea to generate AC or in the finished product AC, one or more activating agents are added according to a certain proportion and uniformly mixed, so that various modified AC varieties with low decomposition temperature can be obtained.
3) A dispersion improving type. In order to overcome the defect that the common AC foaming agent is agglomerated due to electrostatic action to cause agglomeration, inert inorganic compound (such as white carbon black) micro powder is fully mixed with the AC foaming agent as a dispersing aid in production, so that AC particles are partially isolated, the agglomeration possibility is reduced, and agglomeration is avoided in the storage and transportation processes. However, the addition of the dispersant is at the expense of a reduction in the gas evolution of the AC blowing agent. The addition ratio is generally 2% -5%, and the gas evolution of the AC foaming agent can be reduced by 2-3 ml/g.
4) The formation of solid residue is reduced. To reduce the formation of solid residues upon decomposition of the AC blowing agent, metal oxides (e.g., zinc oxide) are added to inhibit the occurrence of secondary reactions upon decomposition of the AC blowing agent, thereby reducing the formation of urazole. Several grades of modified AC blowing agents without settling of solid residues have been developed abroad.
5) Inhibiting foaming. Certain monocarboxylic acids (e.g., maleic acid) and hydrazides thereof (dihydrazide, oxalic acid dihydrazide), amines (3-acetamide), in the presence of a metallic ionic activator, inhibit the decomposition of AC blowing agents. One typical use of inhibitor-containing AC foaming agents is in the production of foamed wallpaper for upholstery.
6) And (4) compounding. One or more foaming agents with specific functions and the AC foaming agent are mixed and compounded, certain efficiency is improved on the basis of not introducing useless impurities, and the method is an effective way for developing modified AC.
The AC series of different plastics and different formulas are developed through modification, the decomposition temperature, the fineness, the gas evolution quantity and the like of the AC foaming agent are required to be different, and the AC special product is required to be produced according to the requirements of customers. Even common AC foaming agents have increasingly high requirements for their exclusive use of gas evolution, fineness and decomposition temperature. The composite foaming agent is developed rapidly, and the foaming agent H, OBSH and the inorganic foaming agent are taken as main bodies, are used together with more than two foaming agents, and are used as an AC foaming agent or matched with other auxiliary agents to meet the requirements of specific application fields. The development trend is that the composite variety of the endothermic and exothermic chemical foaming agent has excellent performance. Dosage form improvement techniques such as improving the dispersibility of the foaming agent and reducing dust pollution are attracting attention, and masterbatch and surface treatment techniques are important issues in current research.
The plastic industry is always seeking a foaming agent product which is convenient to use, safe and reliable, and people are continuously perfecting various performances of the foaming agent for many years, but a good method is not adopted for realizing efficient masterbatch production of the foaming agent all the time, the main problem is that the foaming agent belongs to a heat-sensitive material, the foaming agent is very easy to react in advance during production of masterbatch, even if the product is produced, the dispersion is not uniform during use, the problems of nonuniform foaming and the like of the product are caused, the process for producing the masterbatch is difficult to master, the quality of the product is unstable and the like.
With the continuous development of plastic industry in China, the demand of plastic foaming agent is continuously increased, the quality and standard are continuously close to international standard, and domestic production enterprises also hope to obtain better foaming agent products so as to meet the requirements of producing products.
The foaming agent AC microbead master batch has the advantages of more convenient use, accurate addition, uniform dispersion, safe transportation and storage and the like, can completely meet the requirements of the production process, and obviously improves the production efficiency.
In view of the above, how to overcome the above defects of the conventional foaming agent, and produce a foaming agent with smaller diameter, better fluidity, no dust, no pollution, safe transportation and storage, and convenient use, is a problem to be solved urgently in the industry.
Disclosure of Invention
Aiming at various defects of the traditional foaming agent in the prior art, the invention provides a preparation method of a modified foaming agent microbead master batch.
The invention provides a modified foaming agent microbead master batch which comprises, by weight, 40-300 parts of a foaming agent, 29-75% of an organic carrier material and 2-4 parts of a dispersing agent, wherein the weight ratio of the foaming agent to the organic carrier material is 70-24%.
Preferably, the foaming agent in the modified foaming agent microbead master batch component is an AC foaming agent;
preferably, the organic carrier material in the modified foaming agent microbead master batch component is polyethylene wax or stearic acid;
preferably, the dispersing agent in the modified foaming agent bead master batch is calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene ether phosphate or alkylphenol polyoxyethylene ether phosphate.
The invention also provides a preparation method of the modified foaming agent microbead master batch, which comprises the following steps:
1) adding 100-200 parts by weight of water into a foaming agent and a dispersing agent in a stirring kettle, stirring and mixing uniformly, grinding and circularly dispersing by a colloid mill at the temperature of 60-90 ℃, and dehydrating for later use after completely mixing and refining;
2) heating 100 parts by weight of carrier to 110-125 ℃, adding the carrier into a reaction kettle, keeping the temperature constant, slowly adding 40-300 parts by weight of dehydrated mixture while stirring, keeping the temperature for 1-2 hours, and then preparing a finished product by using centrifugal granulation equipment.
Preferably, the rotational speed of the colloid mill grinding cyclic dispersion in the step 1) of the preparation method of the modified foaming agent microbead master batch is 1700-3500rpm, and the time is 2-3 hours;
preferably, the centrifugal granulation equipment in the step 2) of the preparation method of the modified foaming agent microbead master batch is a centrifugal granulation tower with the length of 5-10 meters;
preferably, the temperature of the centrifugal granulation tower in the step 2) of the preparation method of the modified foaming agent microbead master batch is 10-25 ℃.
The invention has the beneficial effects that:
1) the invention takes the foaming agent as the main part and adds proper dispersant to help the dispersion of the foaming agent. Grinding and refining in water phase by colloid mill, dewatering and separating, coating with organic molecular carrier material, and centrifugal granulating. The technical characteristics are as follows: under the action of dispersant, the foaming agent is dispersed and ground in water phase in a colloid mill to reach particle size not greater than 2 micron. After separation and dehydration, the mixture is mixed and coated with an organic carrier, and the product is obtained through centrifugal granulation. The prepared micro-bead foaming agent has high dispersibility and high compatibility with organic polymer materials. The invention can prepare different system varieties aiming at different materials, has wide application range and is suitable for materials such as rubber, plastic, wood and the like as a foaming agent.
2) The key technology of the invention is the selection of organic carrier materials and a processing method. The technology adopts polyethylene wax or stearic acid as a carrier, the melting point of the carrier is about 90-110 ℃, the carrier is easy to be compatible with most high polymer materials, and simultaneously, various performances of the materials are not influenced. The invention improves the compatibility with synthetic materials, and the technology is not reported in documents at present.
3) The method has the greatest benefits that the AC foaming agent is refined and ground in the water phase by using the colloid mill, and is dispersed, the process is obviously different from the prior process that the foaming agent is refined by adopting airflow pulverization, the safe operability during airflow pulverization is changed, the problems of easy explosion, easy flammability and the like caused by the production of the refined AC foaming agent are completely avoided, and the method has the greatest contribution to improving the production process, storage and transportation safety. The foaming agent and the organic carrier material are fully dispersed and coated under the action of the dispersing agent, and the granulated particles are uniform in size distribution and do not agglomerate. The centrifugal granulation technology is adopted, the spherical structure of the product with the diameter of 0.5-1.0mm is controlled, the flowability is very good, the product is easy to be uniformly mixed with the foaming material, and meanwhile, the centrifugal granulation technology has the advantages of no dust, no pollution, convenience and safety in use and transportation and the like.
Drawings
The various aspects of the present invention will become more apparent to the reader after reading the detailed description of the invention with reference to the attached drawings. Wherein,
figure 1 shows a schematic process flow diagram of the present invention.
Detailed Description
In order to more clearly understand the technical contents of the present invention, embodiments of the present invention are described in further detail below with reference to the accompanying drawings.
The modified foaming agent microbead master batch comprises, by weight, 40-300 parts of a foaming agent, 100 parts of an organic carrier material and 2-4 parts of a dispersing agent, wherein the foaming agent in the modified foaming agent microbead master batch is an AC foaming agent, the organic carrier material is polyethylene wax or stearic acid, the dispersing agent is calcium dodecyl benzene sulfonate or alkylphenol polyoxyethylene ether phosphate, and the dispersing agent adopted in the modified foaming agent microbead master batch is dispersing agent DS-1 and RE-610D-102, so that the dispersing agent can be more easily dispersed in a grinding and refining process.
Figure 1 shows a schematic process flow diagram of the present invention. Referring to FIG. 1, adding water into an AC foaming agent and a dispersing agent in a stirring kettle, stirring and mixing uniformly, wherein the water addition amount is 200 parts by weight, grinding and dispersing by a colloid mill (S1), the reaction conditions are 60-90 ℃, the rotation speed is 1700-3500rpm, after the mixture is refined and mixed completely, mixing, dispersing and coating with a carrier by centrifugal dehydration (S2) (S3-S4), and carrying out centrifugal granulation by a centrifugal granulation tower with the temperature of 5-10 m and the temperature of 10-25 ℃ to obtain a product (S5).
Example 1
10 kg of a commercially available AC foaming agent, 0.2 kg of a calcium dodecylbenzenesulfonate dispersant and 20 kg of water were placed in a 100-liter reaction vessel, stirred and heated, the temperature was controlled at 65 ℃ and held for 1 hour. And circularly dispersing by a colloid mill at the rotating speed of 2000rpm and the temperature of 60-80 ℃, and dehydrating after complete grinding and dispersion. Heating 5 kg of carrier polyethylene wax to 120 ℃, slowly adding the dispersed AC foaming agent under stirring, controlling the temperature at 120 ℃ of 110-120 ℃, keeping the temperature for 1.5 hours, centrifugally granulating, and controlling the diameter of the foaming agent of the product to be spherical with the diameter of 0.5-1.0mm to prepare the modified foaming agent microbead master batch with the foaming agent content of about 65.8 percent.
Example 2
10 kg of a commercial AC foaming agent, 0.2 kg of alkylphenol polyoxyethylene ether phosphate ester dispersing agent and 20 kg of water are put into a 100L reaction kettle, stirred and heated, the temperature is controlled at 65 ℃, and the temperature is kept for 1 hour. And circularly dispersing by a colloid mill under the reaction conditions of 2000rpm and 60-80 ℃, and dehydrating after complete grinding and dispersion. Heating 10 kg of carrier stearic acid to 120 ℃, slowly adding the dispersed AC foaming agent under stirring, keeping the temperature at 120 ℃ for 1.5 hours, centrifugally granulating, and controlling the diameter of the foaming agent product to be 0.5-1.0mm, thus obtaining the modified foaming agent bead master batch with the foaming agent content of about 49.5%.
Therefore, the modified foaming agent microbead master batch disclosed by the invention has high dispersibility and compatibility with an organic polymer material, is uniform in foaming, safe and convenient to use and store, greatly reduces potential safety hazards and environmental hazards due to a processing process, and improves the safety of a foaming agent in transportation, storage and use.
The foregoing describes specific embodiments of the present invention. However, those skilled in the art will appreciate that various modifications and substitutions can be made to the specific embodiments of the present invention without departing from the spirit and scope of the invention. Such modifications and substitutions are intended to be included within the scope of the present invention as defined by the appended claims.
Claims (8)
1. The modified foaming agent microbead master batch is characterized by comprising 40-300 parts of a foaming agent, 100 parts of an organic carrier material and 2-4 parts of a dispersing agent by weight.
2. The modified blowing agent microbead masterbatch of claim 1, wherein the blowing agent is an AC blowing agent.
3. The modified blowing agent microbead masterbatch of claim 1, wherein the organic carrier material is polyethylene wax or stearic acid.
4. The modified blowing agent microbead masterbatch of claim 1, wherein the dispersant is calcium dodecylbenzenesulfonate, alkylphenol ethoxylate phosphate, or alkylphenol ethoxylate phosphate.
5. The preparation method of the modified foaming agent microbead master batch is characterized by comprising the following steps:
1) adding 100-200 parts by weight of water into the foaming agent and the dispersing agent in the stirring kettle according to the claim 1, uniformly stirring and mixing, grinding the circulating water phase by using a colloid mill at the temperature of 60-90 ℃, completely mixing and refining, and dehydrating for later use;
2) heating 100 parts by weight of the carrier of claim 1 to 110-125 ℃, adding the carrier into a reaction kettle, keeping the temperature constant, slowly adding 40-300 parts by weight of the dehydrated mixture in the step 1) while stirring, keeping the temperature for 1-2 hours, and then preparing the finished product by using centrifugal granulation equipment.
6. The method for preparing the modified foaming agent microbead master batch as claimed in claim 5, wherein the rotation speed of the colloid mill grinding circulation dispersion in the step 1) is 1700-3500rpm, and the time is 2-3 hours.
7. The method for preparing a modified foaming agent microbead master batch as claimed in claim 5, wherein the centrifugal granulation equipment in the step 2) is a centrifugal granulation tower with the length of 5-10 meters.
8. The method for preparing a modified blowing agent microbead master batch as claimed in claim 7, wherein the temperature of the centrifugal prilling tower in step 2) is 10-25 ℃.
Priority Applications (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108273455A (en) * | 2018-03-03 | 2018-07-13 | 洛阳和梦科技有限公司 | Ultra-fine high dispersive rubber chemicals process units |
| CN108638610A (en) * | 2018-03-30 | 2018-10-12 | 扬州市腾龙包装材料有限公司 | A kind of cable specific complex protective film and its processing method |
| CN108690241A (en) * | 2018-03-30 | 2018-10-23 | 扬州市腾龙包装材料有限公司 | A kind of photovoltaic glass antistatic fretting map dedicated film and its processing method |
| CN111019184A (en) * | 2019-12-25 | 2020-04-17 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | High-content easily-dispersible foaming master batch and preparation method thereof |
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| CN101838416A (en) * | 2010-02-05 | 2010-09-22 | 上海子元汽车零部件有限公司 | Expandable master batch, expandable material and manufacturing method thereof |
| CN103059391A (en) * | 2011-10-20 | 2013-04-24 | 合肥杰事杰新材料股份有限公司 | Toughened foamed master batch, and preparation method and application thereof |
| CN103289156A (en) * | 2012-02-23 | 2013-09-11 | 苏州井上高分子新材料有限公司 | Uniformly disperse foaming agent masterbatch |
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| CN101838416A (en) * | 2010-02-05 | 2010-09-22 | 上海子元汽车零部件有限公司 | Expandable master batch, expandable material and manufacturing method thereof |
| CN103059391A (en) * | 2011-10-20 | 2013-04-24 | 合肥杰事杰新材料股份有限公司 | Toughened foamed master batch, and preparation method and application thereof |
| CN103289156A (en) * | 2012-02-23 | 2013-09-11 | 苏州井上高分子新材料有限公司 | Uniformly disperse foaming agent masterbatch |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108273455A (en) * | 2018-03-03 | 2018-07-13 | 洛阳和梦科技有限公司 | Ultra-fine high dispersive rubber chemicals process units |
| CN108638610A (en) * | 2018-03-30 | 2018-10-12 | 扬州市腾龙包装材料有限公司 | A kind of cable specific complex protective film and its processing method |
| CN108690241A (en) * | 2018-03-30 | 2018-10-23 | 扬州市腾龙包装材料有限公司 | A kind of photovoltaic glass antistatic fretting map dedicated film and its processing method |
| CN111019184A (en) * | 2019-12-25 | 2020-04-17 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | High-content easily-dispersible foaming master batch and preparation method thereof |
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| CN103351477B (en) | 2015-05-13 |
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