CN105410047A - Method for preparing compound leather mildew-proof bactericidal agent from modified kaolin - Google Patents
Method for preparing compound leather mildew-proof bactericidal agent from modified kaolin Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
- A01N35/06—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing keto or thioketo groups as part of a ring, e.g. cyclohexanone, quinone; Derivatives thereof, e.g. ketals
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/28—Myrtaceae [Myrtle family], e.g. teatree or clove
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Abstract
The invention relates to a method for preparing a compound leather mildew-proof bactericidal agent from modified kaolin, and belongs to the technical field of leather mildew proofness. The method disclosed by the invention comprises the following steps: firstly, activating kaolin at high temperature; then, mixing the activated kaolin with an activating agent and a modifying agent, and amplifying and modifying the interior of the kaolin under high pressure; then, extracting natural mildew-proof bactericidal matter from natural plants, and adsorbing to the modified and activated kaolin; finally, wrapping the kaolin with sodium aliphatate as a protection and slow release agent to obtain the compound leather mildew-proof bactericidal agent. The compound leather mildew-proof bactericidal agent prepared by the method disclosed by the invention has stability, is nontoxic and emits a fresh scent; meanwhile, the compound leather mildew-proof bactericidal agent cannot resist to drugs due to the slow release function of the compound leather mildew-proof bactericidal agent; the compound leather mildew-proof bactericidal agent has long mildew-proof time.
Description
Technical field
The present invention relates to a kind of method preparing composite leather antimildew disinfectant based on modified argil, belong to Leather mildew-proof technical field.
Background technology
Leather is the product of raw hide after de-sheath, tanning processing being rich in collagen, containing protein, grease and various saccharides composition in the raw material used in leather processing procedure, the growth that these materials are mould provides abundant nutrition, the porous of leather and polar structure make its easy moisture absorption, and leather itself is in faintly acid, is the ecotopia of various bacterium fungus growth.The raised growth of mould makes leather go mouldy, and not only affects the attractive in appearance of leather, and serious meeting destroys the quality of leather.
Active component popular in the market has 2-n-octyl-4-isothiazoline-3 ketone (being called for short OIT), molecular structural formula is: be a kind of low toxicity, efficient, broad spectrum type mould inhibitor, to mould, there is very strong killing action, shortcoming is that sulphite can cause it unstable, and Long-Time Service easily develops immunity to drugs, same additive capacity, Leather mildew-proof persistence is shorter and shorter.In addition in Leather mildew-proof technique, the addition of rules and regulations OIT must not more than 100ppm, and in existing leather industry, the addition of 100ppm can not control the amount reproduction of leather contaminated bacteria.Therefore in the urgent need to seeking new leather fungicide.
Summary of the invention
The technical problem that the present invention mainly solves: the existence for the sulphite in the mould inhibitor used at present makes it unstable, to human body, there is harm, and Long-Time Service easily develops immunity to drugs, the problem that mildew-resistant persistence shortens, first the present invention is at high temperature activated by carclazyte, again by the carclazyte after activation and activator and modifier, under high pressure expansion is carried out and modification to carclazyte inside, subsequently extraction Natural anti-mildew Fungicidal substance is carried out to natural plants, and be adsorbed in the carclazyte after modified active, finally use sodium soap as protection and sustained release agent, parcel carclazyte, composite leather antimildew disinfectant can be obtained.Composite leather antimildew disinfectant prepared by the present invention has stability, nontoxic, gives out fragrant, simultaneously its slow releasing effect, and it can not be made to develop immunity to drugs, and the mildew-resistant time is long.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:
(1) get 800 ~ 1200g carclazyte and put into container, add soaked in absolute ethyl alcohol carclazyte wherein, with rotating speed 150 ~ 160r/min, filter after stirring 30 ~ 50min, subsequently the carclazyte after filtration is put into Muffle furnace, design temperature 500 ~ 700 DEG C, insulation activation 20 ~ 30min, then be cooled to room temperature, put into cracker and pulverize, sieve to obtain 120 ~ 150 order treated earth particles;
(2) sodium hydroxide solution being 46% by the carclazyte particle of above-mentioned gained and 400 ~ 600mL mass fraction mixes in glass reaction still, and then add 1 ~ 2g cetyltrimethyl ammonium and 2 ~ 5g neopelex wherein, after mixing, 3 ~ 5MPa is forced into reactor, temperature is set as 55 ~ 65 DEG C, speed setting is 120 ~ 130r/min, slow agitating heating 1 ~ 2h;
(3) discharging after above-mentioned heating terminates, carries out filtration under diminished pressure by the discharging thing of gained, collects filtrate, puts into air-dry machine and carry out air-dry, then it is put into cracker again and pulverize, and crosses standard screen and obtains 200 ~ 300 order modified argil particles, for subsequent use;
(4) by red to ginkgo, Asian puccoon, rosemary, Xue MingRosma rinus officinalis and cloves, mix by quality 1:3:2:1, then mixture is put into baking oven, design temperature is 50 ~ 60 DEG C, keep temperature drying 30 ~ 40min, subsequently mixture is put into cracker and pulverize, sieve to obtain 80 ~ 100 order mixed-powders;
(5) mixed-powder getting the above-mentioned gained of 700 ~ 900g puts into three mouthfuls of round-bottomed flasks, respectively to wherein adding 420 ~ 470mL absolute ethyl alcohol, stir, subsequently beaker is moved in ultrasonic cleaning machine, sonic oscillation 30 ~ 40min, then loads onto reflux in round-bottomed flask, heats until there is drop in reflux condensing tube to flask, keep temperature, backflow 2 ~ 4h;
(6) after above-mentioned backflow terminates, to reduce pressure while hot extracting, collect extract, then by solid-to-liquid ratio 1:2, the modified argil particle of gained in step (3) is mixed with extract, put into container, add the glucolactone of 1 ~ 3% of modified argil granular mass subsequently more wherein, after mixing, container is heated, heating-up temperature is set as 78 ~ 95 DEG C, and heating is until the liquor capacity in container becomes 30 ~ 42% of original solution volume;
(7) after above-mentioned heating terminates, add the sodium soap of 4 ~ 8% of modified argil granular mass wherein, stir until it dissolves completely, leave standstill 1 ~ 2h subsequently, then the mixture in container is put into centrifuge and carry out centrifugation, collect centrifugal thing, carry out natural air drying, composite leather mould inhibitor can be obtained.
Application of the present invention: the composite leather mould inhibitor of above-mentioned preparation is heated, control temperature is 40 ~ 50 DEG C, time is 2 ~ 3min, for subsequent use, again by the leather of required antimycotic antiseptic through chrome tanning, change bath after, being placed in mass fraction is after the hydrochloric acid solution immersion 20 ~ 30min of 30%, the composite leather mould inhibitor 10 ~ 15g after heating is added to it, being placed in temperature is 20 ~ 25 DEG C of process 30 ~ 40min, take out, extension dries in the air, and shears, and adds 10 ~ 15% than traditional mould inhibitor mildew-resistant time.
The invention has the beneficial effects as follows:
(1) composite leather antimildew disinfectant has stability, nontoxic, gives out fragrant;
(2) slow releasing effect, can not develop immunity to drugs, and the mildew-resistant time is long;
(3) preparation process is simple, and cost is low.
Embodiment
First get 800 ~ 1200g carclazyte and put into container, add soaked in absolute ethyl alcohol carclazyte wherein, with rotating speed 150 ~ 160r/min, filter after stirring 30 ~ 50min, subsequently the carclazyte after filtration is put into Muffle furnace, design temperature 500 ~ 700 DEG C, insulation activation 20 ~ 30min, then be cooled to room temperature, put into cracker and pulverize, sieve to obtain 120 ~ 150 order treated earth particles; The sodium hydroxide solution being 46% by the carclazyte particle of above-mentioned gained and 400 ~ 600mL mass fraction again mixes in glass reaction still, and then add 1 ~ 2g cetyltrimethyl ammonium and 2 ~ 5g neopelex wherein, after mixing, 3 ~ 5MPa is forced into reactor, temperature is set as 55 ~ 65 DEG C, speed setting is 120 ~ 130r/min, slow agitating heating 1 ~ 2h; Discharging after above-mentioned heating terminates, carries out filtration under diminished pressure by the discharging thing of gained, collects filtrate, puts into air-dry machine and carry out air-dry, then it is put into cracker again and pulverize, and crosses standard screen and obtains 200 ~ 300 order modified argil particles, for subsequent use; Again by red to ginkgo, Asian puccoon, rosemary, Xue MingRosma rinus officinalis and cloves, mix by quality 1:3:2:1, then mixture is put into baking oven, design temperature is 50 ~ 60 DEG C, keep temperature drying 30 ~ 40min, subsequently mixture is put into cracker and pulverize, sieve to obtain 80 ~ 100 order mixed-powders; Then the mixed-powder getting the above-mentioned gained of 700 ~ 900g puts into three mouthfuls of round-bottomed flasks, respectively to wherein adding 420 ~ 470mL absolute ethyl alcohol, stir, subsequently beaker is moved in ultrasonic cleaning machine, sonic oscillation 30 ~ 40min, then loads onto reflux in round-bottomed flask, heats until there is drop in reflux condensing tube to flask, keep temperature, backflow 2 ~ 4h; After above-mentioned backflow terminates, to reduce pressure while hot extracting, collect extract, then by solid-to-liquid ratio 1:2, modified argil particle is mixed with extract, put into container, add the glucolactone of 1 ~ 3% of modified argil granular mass subsequently more wherein, after mixing, container is heated, heating-up temperature is set as 78 ~ 95 DEG C, and heating is until the liquor capacity in container becomes 30 ~ 42% of original solution volume; After above-mentioned heating terminates, add the sodium soap of 4 ~ 8% of modified argil granular mass wherein, stir until it dissolves completely, leave standstill 1 ~ 2h subsequently, then the mixture in container is put into centrifuge and carry out centrifugation, collect centrifugal thing, carry out natural air drying, composite leather mould inhibitor can be obtained.
Example 1
First get 1200g carclazyte and put into container, add soaked in absolute ethyl alcohol carclazyte wherein, with rotating speed 160r/min, filter after stirring 50min, subsequently the carclazyte after filtration is put into Muffle furnace, design temperature 700 DEG C, insulation activation 30min, then be cooled to room temperature, put into cracker and pulverize, sieve to obtain 150 order treated earth particles; The sodium hydroxide solution being 46% by the carclazyte particle of above-mentioned gained and 600mL mass fraction again mixes in glass reaction still, and then add 2g cetyltrimethyl ammonium and 5g neopelex wherein, after mixing, 5MPa is forced into reactor, temperature is set as 65 DEG C, speed setting is 130r/min, slow agitating heating 2h; Discharging after above-mentioned heating terminates, carries out filtration under diminished pressure by the discharging thing of gained, collects filtrate, puts into air-dry machine and carry out air-dry, then it is put into cracker again and pulverize, and crosses standard screen and obtains 300 order modified argil particles, for subsequent use; Again by red to ginkgo, Asian puccoon, rosemary, Xue MingRosma rinus officinalis and cloves, mix by quality 1:3:2:1, then mixture is put into baking oven, design temperature is 60 DEG C, keep the dry 40min of temperature, subsequently mixture is put into cracker and pulverize, sieve to obtain 100 order mixed-powders; Then the mixed-powder getting the above-mentioned gained of 900g puts into three mouthfuls of round-bottomed flasks, respectively to wherein adding 470mL absolute ethyl alcohol, stir, subsequently beaker is moved in ultrasonic cleaning machine, sonic oscillation 40min, then loads onto reflux in round-bottomed flask, heats until there is drop in reflux condensing tube to flask, keep temperature, backflow 4h; After above-mentioned backflow terminates, to reduce pressure while hot extracting, collect extract, then by solid-to-liquid ratio 1:2, modified argil particle is mixed with extract, put into container, add the glucolactone of 3% of modified argil granular mass subsequently more wherein, after mixing, container is heated, heating-up temperature is set as 95 DEG C, and heating is until the liquor capacity in container becomes 42% of original solution volume; After above-mentioned heating terminates, add the sodium soap of 8% of modified argil granular mass wherein, stir until it dissolves completely, leave standstill 2h subsequently, then the mixture in container is put into centrifuge and carry out centrifugation, collect centrifugal thing, carry out natural air drying, composite leather mould inhibitor can be obtained.The composite leather mould inhibitor of above-mentioned preparation is heated, control temperature is 50 DEG C, and the time is 3min, for subsequent use, again by the leather of required antimycotic antiseptic through chrome tanning, change bath after, be placed in mass fraction be 30% hydrochloric acid solution soak 30min after, add the composite leather mould inhibitor 10g after heating to it, be placed in temperature be 25 DEG C process 40min, take out, extension dries in the air, and shears, and adds 15% than traditional mould inhibitor mildew-resistant time.
Example 2
First get 800g carclazyte and put into container, add soaked in absolute ethyl alcohol carclazyte wherein, with rotating speed 150r/min, filter after stirring 30min, subsequently the carclazyte after filtration is put into Muffle furnace, design temperature 500 DEG C, insulation activation 20min, then be cooled to room temperature, put into cracker and pulverize, sieve to obtain 120 order treated earth particles; The sodium hydroxide solution being 46% by the carclazyte particle of above-mentioned gained and 400mL mass fraction again mixes in glass reaction still, and then add 1g cetyltrimethyl ammonium and 2g neopelex wherein, after mixing, 3MPa is forced into reactor, temperature is set as 55 DEG C, speed setting is 120r/min, slow agitating heating 1h; Discharging after above-mentioned heating terminates, carries out filtration under diminished pressure by the discharging thing of gained, collects filtrate, puts into air-dry machine and carry out air-dry, then it is put into cracker again and pulverize, and crosses standard screen and obtains 200 order modified argil particles, for subsequent use; Again by red to ginkgo, Asian puccoon, rosemary, Xue MingRosma rinus officinalis and cloves, mix by quality 1:3:2:1, then mixture is put into baking oven, design temperature is 50 DEG C, keep the dry 30min of temperature, subsequently mixture is put into cracker and pulverize, sieve to obtain 80 order mixed-powders; Then the mixed-powder getting the above-mentioned gained of 700g puts into three mouthfuls of round-bottomed flasks, respectively to wherein adding 420mL absolute ethyl alcohol, stir, subsequently beaker is moved in ultrasonic cleaning machine, sonic oscillation 30min, then loads onto reflux in round-bottomed flask, heats until there is drop in reflux condensing tube to flask, keep temperature, backflow 2h; After above-mentioned backflow terminates, to reduce pressure while hot extracting, collect extract, then by solid-to-liquid ratio 1:2, modified argil particle is mixed with extract, put into container, add the glucolactone of 1% of modified argil granular mass subsequently more wherein, after mixing, container is heated, heating-up temperature is set as 78 DEG C, and heating is until the liquor capacity in container becomes 30% of original solution volume; After above-mentioned heating terminates, add the sodium soap of 4% of modified argil granular mass wherein, stir until it dissolves completely, leave standstill 1h subsequently, then the mixture in container is put into centrifuge and carry out centrifugation, collect centrifugal thing, carry out natural air drying, composite leather mould inhibitor can be obtained.The composite leather mould inhibitor of above-mentioned preparation is heated, control temperature is 40 DEG C, time is 2min, for subsequent use, then by the leather of required antimycotic antiseptic through chrome tanning, change bath after, be placed in mass fraction be 30% hydrochloric acid solution soak 20min after, add the composite leather mould inhibitor 10g after heating to it, being placed in temperature is 20 DEG C of process 30min, takes out, extension dries in the air, and shears.10% is added than traditional mould inhibitor mildew-resistant time.
Example 3
First get 1000g carclazyte and put into container, add soaked in absolute ethyl alcohol carclazyte wherein, with rotating speed 155r/min, filter after stirring 40min, subsequently the carclazyte after filtration is put into Muffle furnace, design temperature 600 DEG C, insulation activation 25min, then be cooled to room temperature, put into cracker and pulverize, sieve to obtain 130 order treated earth particles; The sodium hydroxide solution being 46% by the carclazyte particle of above-mentioned gained and 500mL mass fraction again mixes in glass reaction still, and then add 1g cetyltrimethyl ammonium and 3g neopelex wherein, after mixing, 4MPa is forced into reactor, temperature is set as 60 DEG C, speed setting is 125r/min, slow agitating heating 1h; Discharging after above-mentioned heating terminates, carries out filtration under diminished pressure by the discharging thing of gained, collects filtrate, puts into air-dry machine and carry out air-dry, then it is put into cracker again and pulverize, and crosses standard screen and obtains 250 order modified argil particles, for subsequent use; Again by red to ginkgo, Asian puccoon, rosemary, Xue MingRosma rinus officinalis and cloves, mix by quality 1:3:2:1, then mixture is put into baking oven, design temperature is 55 DEG C, keep the dry 35min of temperature, subsequently mixture is put into cracker and pulverize, sieve to obtain 90 order mixed-powders; Then the mixed-powder getting the above-mentioned gained of 800g puts into three mouthfuls of round-bottomed flasks, respectively to wherein adding 430mL absolute ethyl alcohol, stir, subsequently beaker is moved in ultrasonic cleaning machine, sonic oscillation 35min, then loads onto reflux in round-bottomed flask, heats until there is drop in reflux condensing tube to flask, keep temperature, backflow 3h; After above-mentioned backflow terminates, to reduce pressure while hot extracting, collect extract, then by solid-to-liquid ratio 1:2, modified argil particle is mixed with extract, put into container, add the glucolactone of 2% of modified argil granular mass subsequently more wherein, after mixing, container is heated, heating-up temperature is set as 90 DEG C, and heating is until the liquor capacity in container becomes 35% of original solution volume; After above-mentioned heating terminates, add the sodium soap of 5% of modified argil granular mass wherein, stir until it dissolves completely, leave standstill 1h subsequently, then the mixture in container is put into centrifuge and carry out centrifugation, collect centrifugal thing, carry out natural air drying, composite leather mould inhibitor can be obtained.The composite leather mould inhibitor of above-mentioned preparation is heated, control temperature is 45 DEG C, and the time is 3min, for subsequent use, again by the leather of required antimycotic antiseptic through chrome tanning, change bath after, be placed in mass fraction be 30% hydrochloric acid solution soak 25min after, add the composite leather mould inhibitor 12g after heating to it, be placed in temperature be 22 DEG C process 35min, take out, extension dries in the air, and shears, and adds 12% than traditional mould inhibitor mildew-resistant time.
Claims (1)
1. prepare a method for composite leather antimildew disinfectant based on modified argil, it is characterized in that concrete preparation process is:
(1) get 800 ~ 1200g carclazyte and put into container, add soaked in absolute ethyl alcohol carclazyte wherein, with rotating speed 150 ~ 160r/min, filter after stirring 30 ~ 50min, subsequently the carclazyte after filtration is put into Muffle furnace, design temperature 500 ~ 700 DEG C, insulation activation 20 ~ 30min, then be cooled to room temperature, put into cracker and pulverize, sieve to obtain 120 ~ 150 order treated earth particles;
(2) sodium hydroxide solution being 46% by the carclazyte particle of above-mentioned gained and 400 ~ 600mL mass fraction mixes in glass reaction still, and then add 1 ~ 2g cetyltrimethyl ammonium and 2 ~ 5g neopelex wherein, after mixing, 3 ~ 5MPa is forced into reactor, temperature is set as 55 ~ 65 DEG C, speed setting is 120 ~ 130r/min, slow agitating heating 1 ~ 2h;
(3) discharging after above-mentioned heating terminates, carries out filtration under diminished pressure by the discharging thing of gained, collects filtrate, puts into air-dry machine and carry out air-dry, then it is put into cracker again and pulverize, and crosses standard screen and obtains 200 ~ 300 order modified argil particles, for subsequent use;
(4) by red to ginkgo, Asian puccoon, rosemary, Xue MingRosma rinus officinalis and cloves, mix by quality 1:3:2:1, then mixture is put into baking oven, design temperature is 50 ~ 60 DEG C, keep temperature drying 30 ~ 40min, subsequently mixture is put into cracker and pulverize, sieve to obtain 80 ~ 100 order mixed-powders;
(5) mixed-powder getting the above-mentioned gained of 700 ~ 900g puts into three mouthfuls of round-bottomed flasks, respectively to wherein adding 420 ~ 470mL absolute ethyl alcohol, stir, subsequently beaker is moved in ultrasonic cleaning machine, sonic oscillation 30 ~ 40min, then loads onto reflux in round-bottomed flask, heats until there is drop in reflux condensing tube to flask, keep temperature, backflow 2 ~ 4h;
(6) after above-mentioned backflow terminates, to reduce pressure while hot extracting, collect extract, then by solid-to-liquid ratio 1:2, the modified argil particle of gained in step (3) is mixed with extract, put into container, add the glucolactone of 1 ~ 3% of modified argil granular mass subsequently more wherein, after mixing, container is heated, heating-up temperature is set as 78 ~ 95 DEG C, and heating is until the liquor capacity in container becomes 30 ~ 42% of original solution volume;
(7) after above-mentioned heating terminates, add the sodium soap of 4 ~ 8% of modified argil granular mass wherein, stir until it dissolves completely, leave standstill 1 ~ 2h subsequently, then the mixture in container is put into centrifuge and carry out centrifugation, collect centrifugal thing, carry out natural air drying, composite leather mould inhibitor can be obtained.
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| CN112376269A (en) * | 2020-11-17 | 2021-02-19 | 国佳新材湖北环保凝胶产业园有限公司 | Aerogel composite fiber felt structural member and preparation method thereof |
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Application publication date: 20160323 |