CN105670028A - Preparation method of conducting foam - Google Patents
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- CN105670028A CN105670028A CN201610208965.9A CN201610208965A CN105670028A CN 105670028 A CN105670028 A CN 105670028A CN 201610208965 A CN201610208965 A CN 201610208965A CN 105670028 A CN105670028 A CN 105670028A
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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Abstract
The invention relates to a preparation method of conducting foam, belonging to the technical field of high-polymer material preparation. The method comprises the following steps: mixing a nickel nitrate solution and a silver nitrate solution, adding urea, dropwisely adding a sodium hydroxide solution, carrying out sealed heating, filtering, drying to obtain a dried mixture, and mixing the dried mixture with calcined carbon black to obtain mixed powder for later use; and pulverizing cleaned wheat straws, mixing the pulverized wheat straws with a foaming agent, a surfactant and the like, foaming by heating, curing by standing, uniformly spreading the mixed powder on the surface of the cured substance, carrying out reduction roasting in a nitrogen/hydrogen atmosphere, cooling by standing, and drying to obtain the conducting foam. The conducting foam has the advantages of stable surface resistivity, stable volume resistivity and long antistatic time (9-10 months).
Description
Technical field
The preparation method that the present invention relates to a kind of conducting foam, belongs to field of polymer material preparing technology.
Background technology
Flame-retardant sponge wraps up conductive fabric, after a series of process, make it have good surface conductivity, can be fixed on readily by adhesive tape needs on shielding device, the shielding material having different section shape, installation method, UL grade and shield effectiveness is available, is widely used in electronic product and military project, the space industries such as PDP TV, LCD display, LCD TV, mobile phone, notebook, MP3, communication cabinet, Medical Instruments.
Current conducting foam mainly has polyethylene or the EVA bulk conducting foam of antistatic PE Foam and moulded from foam, and wherein antistatic PE Foam is because being uncrosslinked polythene material, and he is physical blowing, foam bubble sky is very big, compressive strength is low, and resilience is poor, feel extreme difference, the expansion ratio adding it is single, thickness single error is relatively big, and heatproof is relatively low, and its surface resistivity and specific insulation are unstable, resistivity is relatively big, 108～1011Ω, it is impossible to regulate, it, mainly through adding antistatic additive in PE Foam, makes the PE Foam of antistatic, and this antistatic PE Foam antistatic timeliness is short, and antistatic timeliness is 3～6 months, and antistatic performance is affected bigger by environment humidity. Polyethylene or EVA bulk conducting foam for moulded from foam, although bubble is empty fine and smooth, but mechanical property is poor, and product can not produce continuously, can not be thermally bonded in post-treatment, and have cross-linking agent remaining, abnormal smells from the patient is relatively big, and not environmentally, production efficiency is low.
Summary of the invention
The technical problem to be solved: unstable for antistatic PE Foam and EVA its surface resistivity of bulk conducting foam and specific insulation, resistivity is bigger, cannot regulate, and interpolation antistatic additive, the problem that anti-static effect is short, provide a kind of nickel nitrate solution is mixed with silver nitrate solution after, add carbamide, and drip sodium hydroxide solution, carry out heated sealed, filter, dry, obtain drying composite, and mix with the white carbon black after calcining, obtain mixed-powder, standby, again the wheat stalk cleaned is pulverized, and and foaming agent, the material mixing such as surfactant, foamable, after standing ripening, mixed-powder is uniformly spread on ripening thing surface, under nitrogen and atmosphere of hydrogen, carry out reduction roasting, stand cooling, dry, the method that can obtain conducting foam. conducting foam surface resistivity and specific insulation prepared by the present invention are stable, and antistatic timeliness is long, can maintain 9～10 months.
For solving above-mentioned technical problem, the present invention adopts the technical scheme as described below to be:
(1) 2:1 by volume, by mass fraction be 47% nickel nitrate solution and mass fraction is that 15% silver nitrate solution is uniformly mixed and is placed in container, mixed liquor quality 15～17% carbamide is added again in container, after stirring 15～20min, being slowly added dropwise in container mixture quality 10～12% mass fraction to it is 30% sodium hydroxide solution, and control rate of addition is 1～2mL/min;
(2) after being added dropwise to complete, by seal of vessel, and container is placed in oil bath pan is heated, controlling temperature is 100～140 DEG C, after heating 40～45min, stand and be cooled to room temperature, and it is filtered, it is dry 1～2h in 40～45 DEG C of baking ovens that the filtrate of collection is placed in temperature, can obtain drying composite;
(3) 1～2kg carbon black is weighed, it is placed in calcining furnace and calcines, and after passing into calcining furnace volume 1/3 oxygen in calcining furnace, controlling calcining heat is 200～245 DEG C, calcines 1～2h, after standing is cooled to room temperature, take out, and by the drying composite of extract with above-mentioned preparation after 1:5 is mixed homogeneously in mass ratio, be placed in mill and mill and mistake 150 mesh sieves, obtain mixed-powder, standby;
(4) 1～2kg wheat stalk is weighed, and after rinsing well with clear water, naturally dry, with jet mill, the powder of straw after drying is broken into 70～80 order stalk particles, it is placed in container, in container, add stalk particle quality 2～3% benzene sulfonyl hydrazide and stalk particle quality 3～4% dioctyl sodium sulfosuccinate more respectively, be uniformly mixed;
(5) to be mixed complete after, container is heated being warming up to 70～80 DEG C, heating 40～50min after, adding mixture quality 2～3% polyamide in container again in container, agitating heating is warming up to 85～90 DEG C, after heating 20～30min, standing is cooled to room temperature so that it is ripening 1～2h;
(6) after ripening completes, mixed-powder prepared by step (3) is spread ripening thing surface in container uniformly, and passes into nitrogen in container, after getting rid of the oxygen in container, container volume 1/2 hydrogen is passed into again in container, after having passed into, container being heated, controlling heating-up temperature is 100～110 DEG C, carry out reduction roasting 1～2h, stand again and be cooled to room temperature, and calcining matter is placed in temperature is drying 40～45min in 70～80 DEG C of baking ovens, conducting foam can be prepared into.
Its specific insulation of conducting foam prepared by the present invention is 100～120 Ω cm, and shield effectiveness reaches 60～75dB, and longitudinal tensile strength is 3.05～3.55MPa, and transverse tensile strength is 2.56～2.67MPa, and antistatic can maintain 9～10 months.
The present invention is compared with additive method, and Advantageous Effects is:
(1) conducting foam surface resistivity and the specific insulation that prepared by the present invention are stable, and stability improves 15～17%;
(2) antistatic timeliness is long, can maintain 9～10 months;
(3) the conducting foam big gun hole prepared is fine and smooth, and resilience is good, and feel is submissive, and preparation process is simple, and required cost is low.
Detailed description of the invention
First 2:1 by volume, by mass fraction be 47% nickel nitrate solution and mass fraction is that 15% silver nitrate solution is uniformly mixed and is placed in container, mixed liquor quality 15～17% carbamide is added again in container, after stirring 15～20min, being slowly added dropwise in container mixture quality 10～12% mass fraction to it is 30% sodium hydroxide solution, and control rate of addition is 1～2mL/min;After being added dropwise to complete, by seal of vessel, and container is placed in oil bath pan is heated, controlling temperature is 100～140 DEG C, after heating 40～45min, stand and be cooled to room temperature, and it is filtered, it is dry 1～2h in 40～45 DEG C of baking ovens that the filtrate of collection is placed in temperature, can obtain drying composite; Weigh 1～2kg carbon black again, it is placed in calcining furnace and calcines, and after passing into calcining furnace volume 1/3 oxygen in calcining furnace, controlling calcining heat is 200～245 DEG C, calcines 1～2h, after standing is cooled to room temperature, take out, and by the drying composite of extract with above-mentioned preparation after 1:5 is mixed homogeneously in mass ratio, be placed in mill and mill and mistake 150 mesh sieves, obtain mixed-powder, standby; Weigh 1～2kg wheat stalk, and after rinsing well with clear water, naturally dry, with jet mill, the powder of straw after drying is broken into 70～80 order stalk particles, it is placed in container, in container, add stalk particle quality 2～3% benzene sulfonyl hydrazide and stalk particle quality 3～4% dioctyl sodium sulfosuccinate more respectively, be uniformly mixed; To be mixed complete after, container is heated being warming up to 70～80 DEG C, heating 40～50min after, adding mixture quality 2～3% polyamide in container again in container, agitating heating is warming up to 85～90 DEG C, after heating 20～30min, standing is cooled to room temperature so that it is ripening 1～2h; After ripening completes, the mixed-powder of preparation is spread uniformly ripening thing surface in container, and passes into nitrogen in container, after getting rid of the oxygen in container, container volume 1/2 hydrogen is passed into again in container, after having passed into, container being heated, controlling heating-up temperature is 100～110 DEG C, carry out reduction roasting 1～2h, stand again and be cooled to room temperature, and calcining matter is placed in temperature is drying 40～45min in 70～80 DEG C of baking ovens, conducting foam can be prepared into.
Example 1
First 2:1 by volume, by mass fraction be 47% nickel nitrate solution and mass fraction is that 15% silver nitrate solution is uniformly mixed and is placed in container, mixed liquor quality 17% carbamide is added again in container, after stirring 20min, being slowly added dropwise in container mixture quality 12% mass fraction to it is 30% sodium hydroxide solution, and control rate of addition is 2mL/min; After being added dropwise to complete, by seal of vessel, and container is placed in oil bath pan it is heated, controlling temperature is 140 DEG C, after heating 45min, stands and is cooled to room temperature, and it is filtered, it is dry 2h in 45 DEG C of baking ovens that the filtrate of collection is placed in temperature, can obtain drying composite; Weigh 2kg carbon black again, it is placed in calcining furnace and calcines, and after passing into calcining furnace volume 1/3 oxygen in calcining furnace, controlling calcining heat is 245 DEG C, calcines 2h, after standing is cooled to room temperature, take out, and by the drying composite of extract with above-mentioned preparation after 1:5 is mixed homogeneously in mass ratio, be placed in mill and mill and mistake 150 mesh sieves, obtain mixed-powder, standby; Weigh 2kg wheat stalk, and after rinsing well with clear water, naturally dry, with jet mill, the powder of straw after drying is broken into 80 order stalk particles, it is placed in container, in container, add stalk particle quality 3% benzene sulfonyl hydrazide and stalk particle quality 4% dioctyl sodium sulfosuccinate more respectively, be uniformly mixed; To be mixed complete after, container is heated being warming up to 80 DEG C, after heating 50min, then in container, adds mixture quality 3% polyamide in container, agitating heating is warming up to 90 DEG C, after heating 30min, stands and is cooled to room temperature so that it is ripening 2h;After ripening completes, the mixed-powder of preparation is spread uniformly ripening thing surface in container, and passes into nitrogen in container, after getting rid of the oxygen in container, container volume 1/2 hydrogen is passed into again in container, after having passed into, container being heated, controlling heating-up temperature is 110 DEG C, carry out reduction roasting 2h, stand again and be cooled to room temperature, and calcining matter is placed in temperature is drying 45min in 80 DEG C of baking ovens, conducting foam can be prepared into. Conducting foam surface resistivity and specific insulation prepared by the present invention are stable, and stability improves 17%; Antistatic timeliness is long, can maintain 10 months.
Example 2
First 2:1 by volume, by mass fraction be 47% nickel nitrate solution and mass fraction is that 15% silver nitrate solution is uniformly mixed and is placed in container, mixed liquor quality 15% carbamide is added again in container, after stirring 15min, being slowly added dropwise in container mixture quality 10% mass fraction to it is 30% sodium hydroxide solution, and control rate of addition is 1mL/min; After being added dropwise to complete, by seal of vessel, and container is placed in oil bath pan it is heated, controlling temperature is 100 DEG C, after heating 40min, stands and is cooled to room temperature, and it is filtered, it is dry 1h in 40 DEG C of baking ovens that the filtrate of collection is placed in temperature, can obtain drying composite; Weigh 1kg carbon black again, it is placed in calcining furnace and calcines, and after passing into calcining furnace volume 1/3 oxygen in calcining furnace, controlling calcining heat is 200 DEG C, calcines 1h, after standing is cooled to room temperature, take out, and by the drying composite of extract with above-mentioned preparation after 1:5 is mixed homogeneously in mass ratio, be placed in mill and mill and mistake 150 mesh sieves, obtain mixed-powder, standby; Weigh 1kg wheat stalk, and after rinsing well with clear water, naturally dry, with jet mill, the powder of straw after drying is broken into 70 order stalk particles, it is placed in container, in container, add stalk particle quality 2% benzene sulfonyl hydrazide and stalk particle quality 3% dioctyl sodium sulfosuccinate more respectively, be uniformly mixed; To be mixed complete after, container is heated being warming up to 70 DEG C, after heating 40min, then in container, adds mixture quality 2% polyamide in container, agitating heating is warming up to 85 DEG C, after heating 20min, stands and is cooled to room temperature so that it is ripening 1h; After ripening completes, the mixed-powder of preparation is spread uniformly ripening thing surface in container, and passes into nitrogen in container, after getting rid of the oxygen in container, container volume 1/2 hydrogen is passed into again in container, after having passed into, container being heated, controlling heating-up temperature is 100 DEG C, carry out reduction roasting 1h, stand again and be cooled to room temperature, and calcining matter is placed in temperature is drying 40min in 70 DEG C of baking ovens, conducting foam can be prepared into. Conducting foam surface resistivity and specific insulation prepared by the present invention are stable, and stability improves 15%; Antistatic timeliness is long, can maintain 9 months.
Example 3
First 2:1 by volume, by mass fraction be 47% nickel nitrate solution and mass fraction is that 15% silver nitrate solution is uniformly mixed and is placed in container, mixed liquor quality 16% carbamide is added again in container, after stirring 17min, being slowly added dropwise in container mixture quality 11% mass fraction to it is 30% sodium hydroxide solution, and control rate of addition is 1mL/min; After being added dropwise to complete, by seal of vessel, and container is placed in oil bath pan it is heated, controlling temperature is 120 DEG C, after heating 42min, stands and is cooled to room temperature, and it is filtered, it is dry 1h in 42 DEG C of baking ovens that the filtrate of collection is placed in temperature, can obtain drying composite;Weigh 2kg carbon black again, it is placed in calcining furnace and calcines, and after passing into calcining furnace volume 1/3 oxygen in calcining furnace, controlling calcining heat is 230 DEG C, calcines 2h, after standing is cooled to room temperature, take out, and by the drying composite of extract with above-mentioned preparation after 1:5 is mixed homogeneously in mass ratio, be placed in mill and mill and mistake 150 mesh sieves, obtain mixed-powder, standby; Weigh 1kg wheat stalk, and after rinsing well with clear water, naturally dry, with jet mill, the powder of straw after drying is broken into 75 order stalk particles, it is placed in container, in container, add stalk particle quality 3% benzene sulfonyl hydrazide and stalk particle quality 3% dioctyl sodium sulfosuccinate more respectively, be uniformly mixed; To be mixed complete after, container is heated being warming up to 75 DEG C, after heating 45min, then in container, adds mixture quality 3% polyamide in container, agitating heating is warming up to 87 DEG C, after heating 25min, stands and is cooled to room temperature so that it is ripening 2h; After ripening completes, the mixed-powder of preparation is spread uniformly ripening thing surface in container, and passes into nitrogen in container, after getting rid of the oxygen in container, container volume 1/2 hydrogen is passed into again in container, after having passed into, container being heated, controlling heating-up temperature is 105 DEG C, carry out reduction roasting 1h, stand again and be cooled to room temperature, and calcining matter is placed in temperature is drying 42min in 80 DEG C of baking ovens, conducting foam can be prepared into. Conducting foam surface resistivity and specific insulation prepared by the present invention are stable, and stability improves 16%; Antistatic timeliness is long, can maintain 9 months.
Claims (1)
1. the preparation method of a conducting foam, it is characterised in that concrete preparation process is:
(1) 2:1 by volume, by mass fraction be 47% nickel nitrate solution and mass fraction is that 15% silver nitrate solution is uniformly mixed and is placed in container, mixed liquor quality 15～17% carbamide is added again in container, after stirring 15～20min, being slowly added dropwise in container mixture quality 10～12% mass fraction to it is 30% sodium hydroxide solution, and control rate of addition is 1～2mL/min;
(2) after being added dropwise to complete, by seal of vessel, and container is placed in oil bath pan is heated, controlling temperature is 100～140 DEG C, after heating 40～45min, stand and be cooled to room temperature, and it is filtered, it is dry 1～2h in 40～45 DEG C of baking ovens that the filtrate of collection is placed in temperature, can obtain drying composite;
(3) 1～2kg carbon black is weighed, it is placed in calcining furnace and calcines, and after passing into calcining furnace volume 1/3 oxygen in calcining furnace, controlling calcining heat is 200～245 DEG C, calcines 1～2h, after standing is cooled to room temperature, take out, and by the drying composite of extract with above-mentioned preparation after 1:5 is mixed homogeneously in mass ratio, be placed in mill and mill and mistake 150 mesh sieves, obtain mixed-powder, standby;
(4) 1～2kg wheat stalk is weighed, and after rinsing well with clear water, naturally dry, with jet mill, the powder of straw after drying is broken into 70～80 order stalk particles, it is placed in container, in container, add stalk particle quality 2～3% benzene sulfonyl hydrazide and stalk particle quality 3～4% dioctyl sodium sulfosuccinate more respectively, be uniformly mixed;
(5) to be mixed complete after, container is heated being warming up to 70～80 DEG C, heating 40～50min after, adding mixture quality 2～3% polyamide in container again in container, agitating heating is warming up to 85～90 DEG C, after heating 20～30min, standing is cooled to room temperature so that it is ripening 1～2h;
(6) after ripening completes, mixed-powder prepared by step (3) is uniformly spread to the ripening thing surface in container, and in container, passes into nitrogen, after getting rid of the oxygen in container, container volume 1/2 hydrogen is passed into again in container, after having passed into, container being heated, controlling heating-up temperature is 100～110 DEG C, carry out reduction roasting 1～2h, stand again and be cooled to room temperature, and calcining matter is placed in temperature is drying 40～45min in 70～80 DEG C of baking ovens, conducting foam can be prepared into.
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| CN106009578A (en) * | 2016-07-02 | 2016-10-12 | 郭迎庆 | Preparation method for acetylated lignin-modified unsaturated polyester conductive foam |
| CN106297965A (en) * | 2016-08-16 | 2017-01-04 | 苏州市云林电子有限公司 | A kind of multilayer conductive foam |
| CN111148012A (en) * | 2019-12-02 | 2020-05-12 | 苏州市新广益电子有限公司 | Conductive foam for loudspeaker and electronic terminal equipment and production process thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106009578A (en) * | 2016-07-02 | 2016-10-12 | 郭迎庆 | Preparation method for acetylated lignin-modified unsaturated polyester conductive foam |
| CN106297965A (en) * | 2016-08-16 | 2017-01-04 | 苏州市云林电子有限公司 | A kind of multilayer conductive foam |
| CN111148012A (en) * | 2019-12-02 | 2020-05-12 | 苏州市新广益电子有限公司 | Conductive foam for loudspeaker and electronic terminal equipment and production process thereof |
| CN111148012B (en) * | 2019-12-02 | 2020-12-29 | 苏州市新广益电子有限公司 | Conductive foam for loudspeaker and electronic terminal equipment and production process thereof |
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