CN104960129A - Preparation method of flexible silica-based gamma shielding composite roll-type film - Google Patents
Preparation method of flexible silica-based gamma shielding composite roll-type film Download PDFInfo
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- CN104960129A CN104960129A CN201510312772.3A CN201510312772A CN104960129A CN 104960129 A CN104960129 A CN 104960129A CN 201510312772 A CN201510312772 A CN 201510312772A CN 104960129 A CN104960129 A CN 104960129A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
- B29C43/24—Calendering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/88—Adding charges, i.e. additives
- B29B7/90—Fillers or reinforcements, e.g. fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Thermal Sciences (AREA)
- Laminated Bodies (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a preparation method of a flexible silica-based gamma shielding composite roll-type film. The preparation method is characterized in that high-temperature vulcanization type silicone rubber and a gamma shielding functional filler serving as raw materials, and a platinum vulcanizing agent serving an auxiliary agent are plastified in an open mill, and pretreated by a cationic antistatic agent; the materials after the pretreatment are sent to a rolling device and rolled with a polyester film to form a composite film; and the composite film is subjected to atmospheric pressure vulcanization and winding by a constant temperature tunnel oven to form the flexible silica-based gamma shielding composite roll-type film. The preparation method only requires once open type vulcanization; a vulcanizing speed is controllable; the roll-type silicone rubber film with uniform thickness and width can be continuously produced; the preparation method is simple to operate, improves the production efficiency and can also save the production cost; and different flexible shielding materials with the antistatic property can be prepared by the method as required, and can adapt to different environments.
Description
Technical field
The present invention relates to the preparing technical field of Shielding Materials for Nuclear Radiation, particularly relate to a kind of preparation method of flexible silicon matrix gamma shielding composite rolling film.
Background technology
Along with the develop rapidly of economy, nuclear technology plays increasing effect in the field such as national defense and military, medical diagnosis, industrial production.But due to the existence of nuclear radiation, also bring certain harm also to people, need the research and development carrying out shielding material for this reason, ensure the health of human body of practitioner.
A kind of linear polymeric material made by silicon rubber, and compliance is good, has excellent heat endurance, weatherability, tearing toughness, excellent thermal diffusivity and caking property etc. after over cure, is suitable as matrix material research and development novel flexible shielding material.
Traditional processing mode generally for the rubber-based shielding material of flexibility can be divided into three kinds substantially, and namely hot-forming, injection mo(u)lding and hot-air add sulphur.The mode then mainly adopting hot-forming and hot-air to add sulphur when producing sheet film material is carried out, and the defect of existence is mainly: thermoforming way speed of production is slow, and cannot continuous seepage.Therefore, be necessary to develop a kind of can rapid shaping and can the production technology of quantity-produced rolling flexible shielding material film, promote novel flexible material shielding material extension application.
Summary of the invention
For above-mentioned Problems existing, the object of the invention is to provide that a kind of step is simple, usage range wide, have the process for producing of the flexible silicone rubber base gamma shielding material rolling film of certain antistatic property.
In order to achieve the above object, the technical solution used in the present invention is as follows: a kind of preparation method of flexible silicon matrix gamma shielding composite rolling film, described preparation method is with high temperature vulcanizable silicone and gamma shielding functional stuffing raw material, with platinum vulcanizing agent for auxiliary agent is plasticated in mill, pretreatment is carried out by cationic antistatic agent, pretreated material feeding calender device and polyester film are carried out calendering and obtains laminated film, through constant temperature tunnel type baking oven atmospheric pressure vulcanization, rolling, obtain flexible silicon matrix gamma shielding composite rolling film; Its detailed production stage is as follows:
1) mixing: high temperature vulcanizate is plasticated on a mill until, time is 5 ~ 10min, temperature is 30 ~ 40 DEG C. then adds platinum vulcanizing agent B component and to plasticate 10 ~ 15min, add platinum vulcanizing agent A component again and continue the 10 ~ 15min that plasticates, finally add gamma shielding functional stuffing, temperature maintains 105 ~ 115 DEG C, and mixing time is 20 ~ 30min, obtains flexible silicone rubber base shielding material film;
2) pretreatment: carry out coating operation respectively with the contact surface of the cationic antistatic agent of water white transparency shape to the flexible silicone rubber base shielding material film in polyester film and step 1) on coating machine, coating thickness is 30 ~ 50 um, obtains pretreated flexible silicone rubber base shielding material film mixture and pretreated polyester film;
3) masking is rolled: by step 2) de-bubble of gained pretreated flexible silicone rubber base shielding material film mixture feeding extruder, again with step 2) in send into calender together with pretreated polyester film and carry out calendering and obtain silicone rubber based shielding material polyester compound film, during calendering, temperature controls at 60 ~ 80 DEG C;
4) sulfuration: silicone rubber based for step 3) gained shielding material polyester compound film sent in constant temperature tunnel type baking oven, carry out atmospheric pressure vulcanization, controls curing temperature 150 ~ 170 DEG C, and to control its time of staying in constant temperature tunnel type baking oven be 8 ~ 15min;
5) rolling: by the flexible silicone rubber base shielding material film that obtains in step 4) through wind-up operation, obtain silicone rubber based shielding material film.
Step 2 of the present invention) in water white transparency shape cationic antistatic agent in the parts by weight of each component as follows: polychlorostyrene dihydroxy ethyl-2 hydroxypropyl ammonium chloride 20 ~ 40 parts, butyl acrylate 1.5 ~ 5 parts, styrene 1.5 ~ 5 parts, peroxycarbonates 0.6 ~ 1.5 part, absolute ethyl alcohol 50 ~ 70 parts, peroxidating two alkane initator 0.5 part.
The production method of the cationic antistatic agent of water white transparency shape of the present invention is as follows: each component in being filled a prescription by cationic antistatic agent is under 75 DEG C of conditions, and stirring reaction 8h, cooling obtains water white transparency glue solution of sticky shape gradually.
Platinum vulcanizing agent A component of the present invention is mainly the complex compound of chloroplatinic acid and siloxanes, and platinum vulcanizing agent B component is mainly the mixture of delayed-action activator and hydrogen-containing siloxane crosslinking agent.
The material of polyester film of the present invention is PETG.
Before the wind-up operation of step 4) of the present invention, need the polyester film of flexible silicone rubber base shielding material polyester compound film step 3) obtained to tear, obtain flexible silicone rubber base shielding material film and proceed wind-up operation.
The invention has the advantages that: the production technology of gained flexible silicone rubber base shielding material rolling film of the present invention, only once openly need add sulphur, curingprocess rate is controlled, and can continuous seepage membrane, then thickness and the homogeneous silicon rubber film coil of fabric width can be produced through the sulfuration of constant temperature tunnel type baking oven; The step of explained hereafter is few, simple to operation, the production cost of enterprise reduced while improving the production efficiency of enterprise; What process for producing of the present invention just can produce different size according to actual needs through simple adjustment in addition has anlistatig flexible silicone rubber base volume formula film, can meet the requirement of high-accuracy electronic instrument to the antistatic property of flexible shielding material.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail.
embodiment 1:a kind of preparation method of flexible silicon matrix gamma shielding composite rolling film:
1) mixing: first the high temperature vulcanizate of 100g to be plasticated on a mill until, after 5 minutes, add 1.5g platinum vulcanizing agent B component to plasticate 10 minutes, add 0.5g platinum vulcanizing agent A component again to continue to plasticate 10 minutes, finally by mixing for the 400g gamma shielding functional stuffing of modification enter material, temperature is regulated to be 105 DEG C, mixing 20 minutes.
2) pretreatment: the surface combined with flexible silicone rubber base to PETG film applies the cationic antistatic agent of viscosity and thickness is 30um, wherein, described antistatic additive is by polychlorostyrene dihydroxy ethyl-2 hydroxypropyl ammonium chloride 20%, butyl acrylate 1.5%, styrene 1.5%, peroxycarbonates 1.5%, absolute ethyl alcohol 75%, and the peroxidating two alkane initator of 0.5%, under 75 DEG C of conditions, stirring reaction 8h, cooling obtains water white transparency glue solution of sticky shape gradually.
3) roll film forming: step (1) gained new type silicone rubber base shielding material mixture is sent into extruder de-bubble, then send into calender carry out calendering and obtain silicone rubber based shielding material polyester compound film together with polyester film, during calendering, temperature controls at 60 DEG C.
4) sulfuration: silicone rubber based for step (2) gained shielding material polyester compound film is sent in constant temperature tunnel type baking oven, carry out atmospheric pressure vulcanization, and the antistatic additive between polyester film and flexible silicone rubber base shielding material film is cured simultaneously, constant temperature tunnel type baking oven temperature is set to 150 DEG C, and to control the described flexible silicone rubber base shielding material polyester compound film time rested in baking oven be 8 minutes.
After sulfuration, the polyester film of flexible silicone rubber of tearing base shielding material composite film surface.
5) rolling obtains described flexible silicone rubber base shielding material film.
The surface resistivity of more than obtained flexible silicone rubber base shielding material rolling film is 3.1 × 10
9Ω cm, has certain antistatic property, may be used for the dust-proof pollution of accurate radiation detection instrument.
embodiment 2:a kind of preparation method of flexible silicon matrix gamma shielding composite rolling film:
1) mixing: first the high temperature vulcanizate of 100g to be plasticated on a mill until, after 8 minutes, add 1.5g platinum vulcanizing agent B component to plasticate 12 minutes, add 0.5g platinum vulcanizing agent A component again to continue to plasticate 12 minutes, finally by mixing for the 400g gamma shielding functional stuffing of modification enter material, temperature is regulated to be 110 DEG C, mixing 25 minutes.
2) pretreatment: the surface combined with flexible silicone rubber base to PETG film applies the cationic antistatic agent of viscosity and thickness is 40um, wherein, described antistatic additive is by polychlorostyrene dihydroxy ethyl-2 hydroxypropyl ammonium chloride 30%, butyl acrylate 3%, styrene 3%, peroxycarbonates 1%, absolute ethyl alcohol 62.5%, and 0.5% peroxidating two alkane initator, under 75 DEG C of conditions, stirring reaction 8h, cooling obtains water white transparency glue solution of sticky shape gradually.
3) roll film forming: step (1) gained new type silicone rubber base shielding material mixture is sent into extruder de-bubble, then send into calender carry out calendering and obtain silicone rubber based shielding material polyester compound film together with polyester film, during calendering, temperature controls at 70 DEG C.
4) sulfuration: silicone rubber based for step (2) gained shielding material polyester compound film is sent in constant temperature tunnel type baking oven, carry out atmospheric pressure vulcanization, and the antistatic additive between polyester film and flexible silicone rubber base shielding material film is cured simultaneously, constant temperature tunnel type baking oven temperature is set to 170 DEG C, and to control the described flexible silicone rubber base shielding material polyester compound film time rested in baking oven be 12 minutes.
After sulfuration, the polyester film of flexible silicone rubber of tearing base shielding material composite film surface.
5) rolling obtains described flexible silicone rubber base shielding material film.
The surface resistivity of more than obtained flexible silicone rubber base shielding material rolling film is 2.6 × 10
8Ω cm, antistatic property is better, may be used for the interference protection material of electronic instrument surface radiation proof and electrostatic.
embodiment 3:a kind of preparation method of flexible silicon matrix gamma shielding composite rolling film:
1) mixing: first the high temperature vulcanizate of 100g to be plasticated on a mill until, after 10 minutes, add 1.5g platinum vulcanizing agent B component to plasticate 15 minutes, add 0.5g platinum vulcanizing agent A component again to continue to plasticate 15 minutes, finally by mixing for the 400g gamma shielding functional stuffing of modification enter material, temperature is regulated to be 115 DEG C, mixing 30 minutes.
2) pretreatment: the surface combined with flexible silicone rubber base to PETG film applies the cationic antistatic agent of viscosity and thickness is 50um, wherein, described antistatic additive is by polychlorostyrene dihydroxy ethyl-2 hydroxypropyl ammonium chloride 40%, butyl acrylate 5%, styrene 5%, peroxycarbonates 1.5%, absolute ethyl alcohol 48%, and the peroxidating two alkane initator of 0.5%, under 75 DEG C of conditions, stirring reaction 8h, cooling obtains water white transparency glue solution of sticky shape gradually.
3) roll film forming: step (1) gained new type silicone rubber base shielding material mixture is sent into extruder de-bubble, then send into calender carry out calendering and obtain silicone rubber based shielding material polyester compound film together with polyester film, during calendering, temperature controls at 80 DEG C.
4) sulfuration: silicone rubber based for step (2) gained shielding material polyester compound film is sent in constant temperature tunnel type baking oven, carry out atmospheric pressure vulcanization, and the antistatic additive between polyester film and flexible silicone rubber base shielding material film is cured simultaneously, constant temperature tunnel type baking oven temperature is set to 180 DEG C, and to control the described flexible silicone rubber base shielding material polyester compound film time rested in baking oven be 15 minutes.
After sulfuration, the polyester film of flexible silicone rubber of tearing base shielding material composite film surface.
5) rolling obtains described flexible silicone rubber base shielding material film.
The surface resistivity of more than obtained flexible silicone rubber base shielding material rolling film is 1.2 × 10
7Ω cm, antistatic property is superior, can be used as radiation protection system of mourning and makes material, ensures the comfortable of human body.
embodiment 4:contrast test; When other working conditions and composition of raw materials inconvenience, the different working condition in production technology is carried out contrast test, if shown in its structure following table:
Can be learnt by upper table, in production process of the present invention, the consumption of antistatic additive and thickness can affect the antistatic property of final products, when the consumption of antistatic additive increases gradually, the sheet resistance of final products is caused to decline, and then promote the overall performance of final products, but when its consumption is too much, although the performance boost of its final products, but the thickness of the finished product produced and weight also corresponding increase, be unfavorable for the further production of film product, shorten its range of application, sheet resistance simultaneously in prescribed limit can be applied to most production, too high antistatic property is also impracticable, the consumption of very few antistatic additive then significantly reduces the antistatic property of final products, and practical function is poor.
embodiment 5:carry out contrast test to the formula consumption of component each in the present invention under the same conditions, its experimental result is as shown in the table:
Can be learnt by upper table: in production process of the present invention, the materials of high temperature vulcanizate and gamma shielding functional stuffing are than being fixing, the character that all can affect the sheet resistance of final products of too much high temperature vulcanizate or gamma shielding material, the consumption of gamma shielding functional stuffing is not easily too much, too much consumption then affects the melting effect of itself and high temperature vulcanizate, the main performance of final products can not be improved, cause unnecessary waste, very few consumption then can affect the gamma-ray function of shielding of final products; In platinum vulcanizing agent, the consumption of each component can affect molding effect and the uniformity of mixing product simultaneously, is unfavorable for the aftertreatment technology of product.
It should be noted that, above-mentioned is only preferred embodiment of the present invention, is not used for limiting protection scope of the present invention, and equivalents done on the basis of above-described embodiment all belongs to protection scope of the present invention.
Claims (6)
1. the preparation method of a flexible silicon matrix gamma shielding composite rolling film, it is characterized in that, described preparation method is with 100 parts of high temperature vulcanizable silicones and 400 parts of gamma shielding functional stuffing raw materials, with 1 ~ 2.5 part of platinum vulcanizing agent for auxiliary agent is plasticated in mill, pretreatment is carried out by cationic antistatic agent, pretreated material feeding calender device and polyester film are carried out calendering and obtains laminated film, through constant temperature tunnel type baking oven atmospheric pressure vulcanization, rolling, obtain flexible silicon matrix gamma shielding composite rolling film; Its detailed production stage is as follows:
1) mixing: high temperature vulcanizate is plasticated on a mill until, time is 5 ~ 10min, temperature is 30 ~ 40 DEG C. then adds platinum vulcanizing agent B component and to plasticate 10 ~ 15min, add platinum vulcanizing agent A component again and continue the 10 ~ 15min that plasticates, finally add gamma shielding functional stuffing, temperature maintains 105 ~ 115 DEG C, and mixing time is 20 ~ 30min, obtains flexible silicone rubber base shielding material film;
2) pretreatment: carry out coating operation respectively with the contact surface of the cationic antistatic agent of water white transparency shape to the flexible silicone rubber base shielding material film in polyester film and step 1) on coating machine, obtain pretreated flexible silicone rubber base shielding material film mixture and pretreated polyester film;
3) masking is rolled: by step 2) de-bubble of gained pretreated flexible silicone rubber base shielding material film mixture feeding extruder, again with step 2) in send into calender together with pretreated polyester film and carry out calendering and obtain silicone rubber based shielding material polyester compound film, during calendering, temperature controls at 60 ~ 80 DEG C;
4) sulfuration: silicone rubber based for step 3) gained shielding material polyester compound film sent in constant temperature tunnel type baking oven, carry out atmospheric pressure vulcanization, controls curing temperature 150 ~ 170 DEG C, and to control its time of staying in constant temperature tunnel type baking oven be 8 ~ 15min;
5) rolling: by the flexible silicone rubber base shielding material film that obtains in step 4) through wind-up operation, obtain silicone rubber based shielding material film.
2. the preparation method of flexible silicon matrix gamma shielding composite rolling film according to claim 1, it is characterized in that, described step 2) in water white transparency shape cationic antistatic agent in the parts by weight of each component as follows: polychlorostyrene dihydroxy ethyl-2 hydroxypropyl ammonium chloride 20 ~ 40 parts, butyl acrylate 1.5 ~ 5 parts, styrene 1.5 ~ 5 parts, peroxycarbonates 0.6 ~ 1.5 part, absolute ethyl alcohol 50 ~ 70 parts, peroxidating two alkane initator 0.5 part.
3. the preparation method of flexible silicon matrix gamma shielding composite rolling film according to claim 2, it is characterized in that, the production method of the cationic antistatic agent of described water white transparency shape is as follows: each component in being filled a prescription by cationic antistatic agent is under 75 DEG C of conditions, stirring reaction 8h, cooling obtains water white transparency glue solution of sticky shape gradually.
4. the preparation method of flexible silicon matrix gamma shielding composite rolling film according to claim 1, it is characterized in that, described platinum vulcanizing agent A component is the complex compound of chloroplatinic acid and siloxanes, and platinum vulcanizing agent B component is the mixture of delayed-action activator and siloxane crosslinker.
5. the preparation method of flexible silicon matrix gamma shielding composite rolling film according to claim 1, it is characterized in that, the material of described polyester film is PETG.
6. the preparation method of flexible silicon matrix gamma shielding composite rolling film according to claim 1, it is characterized in that, before the wind-up operation of described step 4), need the polyester film of flexible silicone rubber base shielding material polyester compound film step 3) obtained to tear, obtain flexible silicone rubber base shielding material film and proceed wind-up operation.
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| CN107033472A (en) * | 2017-05-24 | 2017-08-11 | 北京市射线应用研究中心 | A kind of self-adhering-type gamma-rays rubber composite shielding material and preparation method and application |
| CN107082965A (en) * | 2017-05-24 | 2017-08-22 | 北京市射线应用研究中心 | A kind of anti-neutron composite shielding material of self-adhering-type and preparation method and application |
| CN114536799A (en) * | 2022-02-23 | 2022-05-27 | 宁波腾燊科技发展有限公司 | Production equipment and production method of ultra-high molecular weight polyethylene composite membrane |
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| CN114536799A (en) * | 2022-02-23 | 2022-05-27 | 宁波腾燊科技发展有限公司 | Production equipment and production method of ultra-high molecular weight polyethylene composite membrane |
| CN114536799B (en) * | 2022-02-23 | 2024-05-24 | 宁波腾燊科技发展有限公司 | Production equipment and production method of ultra-high molecular weight polyethylene composite film |
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| CN104960129B (en) | 2017-08-25 |
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