CN102795949B - Smokeless cellulose - Google Patents
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- CN102795949B CN102795949B CN201210334268.XA CN201210334268A CN102795949B CN 102795949 B CN102795949 B CN 102795949B CN 201210334268 A CN201210334268 A CN 201210334268A CN 102795949 B CN102795949 B CN 102795949B
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Abstract
The invention discloses a smokeless cellulose which is used for preparing fireworks. The smokeless cellulose is a solid-state micropowder or particle agent. The invention is characterized in that the smokeless cellulose is prepared by nitrating plant fiber and comprises the following components in parts by weight: 100 parts of plant fiber, 40-80 parts of 60-98% nitric acid, 10-50 parts of 60-98% sulfuric acid, 0.5-5 parts of diphenylamine, 0.5-5 parts of camphor, 1-10 parts of sodium carbonate and 50-100 parts of solvent, wherein the plant fiber is one or mixture of pulverized corn cob, corn stalk, bamboo, boon, peanut shell, reed and sugar cane waste residue in any weight ratio; the mixture of nitric acid and sulfuric acid is used as a nitrating agent; the mixture of diphenylamine and camphor is used as a stabilizer; and the solvent is alcohol, banana oil, aether or acetone. The invention has the advantages of high safety, high stability, no smoke, no smell, no toxicity, no dust, environmental protection and the like.
Description
Technical field
The present invention relates to a kind of for preparing the quick-fried medicament of firworks string, especially relating to a kind of smokeless Mierocrystalline cellulose.
Background technology
The quick-fried production history having more than one thousand years in China of firworks string, its product produced sets off band, and to give people incomparable happy and lucky, also band gives considerable Social and economic benef@simultaneously, but manufacturing enterprise has also paid huge life and property loss for this reason, be mainly manifested in the production of firework product and storage and transport process because the casualty accident caused of exploding happens occasionally, one of them important reason be produce the quick-fried drug material friction sensitivity of firworks string and impact sensitivity high, when compounding pharmaceutical mixes by craft or machinery due to friction or shock, very easily to blast casualty accident, in production with to use and very dangerous in transporting.Although at present institute uses the main raw material preparing firework product to have oxidation susceptibility is good, inflammableness and the feature such as explosiveness is strong, produce more dense smoke during owing to setting off, not only affect and set off visual effect, and serious environment pollution.
At present, develop to high-performance environment-friendly safety type along with environmental requirement with to the quick-fried inherent medicine of firworks string, product is to the form development such as indoor, smokeless, the quick-fried manufacturing enterprise of firworks string produces a large amount of smog to reduce to set off, improve the visual effect that product is seted off, in the different agents of many products, use expired rifle, the shell single-base powder scrapped of military project, as propelling charge, ignition powder, open the preparation of luxuriant medicine, spraying decoration medicine etc.Although single-base powder can reduce a large amount of smog in firework product, because single-base powder belongs to military control, unsuitable civilian popularization, and supply limited, on the high side, product cost is increased, and the supply quantity of existing smokeless gun propellant cannot meet the needs of the quick-fried production of firworks string.Upgrade for this reason and manufacture the necessary and prospect of a kind of firworks string that is safe, efficient, environment-friendly type quick-fried novel material medicament with exploitation.
Summary of the invention
The object of the invention is for the firworks string known quick-fried application conventional medicament material technology Problems existing, on the basis of existing pharmaceutical formulation techniques, research trial has repeatedly been carried out to can be used as the quick-fried drug material of firworks string, wish to overcome existing firework powder manufacture easily to blast accident, for preparing the shortcoming that when firework product is seted off, cigarette thickness is dense, by technological innovation and integration, and provide a kind of for preparing the quick-fried smokeless Mierocrystalline cellulose of firworks string, this smokeless Mierocrystalline cellulose preparation technology is easy, security is high, shock resistance, the ability of friction and high pressure is strong, physics stability and chemical stability good, firework display effect is better, the feature that rate of moisture absorption is low and cost is low, and it is smokeless, dustless, tasteless, nontoxic, safety, environmental protection, meet country about the quick-fried safety standards of firworks string, the propelling charge of various firework product or ignition powder can be widely used in or open the needs of the preparation such as luxuriant medicine or spraying decoration medicine.
Object of the present invention can be realized by following technical solution:
A kind of smokeless Mierocrystalline cellulose, quick-fried for preparing firworks string, be solid-state micro mist shape or microgranular medicament, its special character is, it is made through nitrating agent nitration reaction by vegetable fibre, and its component and ratio of weight and number are:
Vegetable fibre: refer to the corn cob through pulverizing, corn stalk, bamboo wood, waste of flax, Pericarppium arachidis hypogaeae, reed, sugarcane waste residue, wherein any one or multiple any ratio of weight and number mixture, consumption is 100 weight parts;
Nitrating agent: described nitrating agent is nitric acid and sulfuric acid mixture, wherein concentration of nitric acid is 60-98%, and consumption is 40-80 weight part, and sulfuric acid concentration is 60-98%, and consumption is 10-50 weight part;
Stablizer: described stablizer is the mixture of pentanoic and camphor, consumption is pentanoic 0.5-5 weight part, camphor 0.5-5 weight part.
Soda ash: consumption is 1-10 weight part;
Solvent: the wherein one of alcohol or lacquer thinner or ether or acetone, consumption is 50-100 weight part.
Smokeless Mierocrystalline cellulose of the present invention, be equipped with standby 100 weight part vegetable fibres, preferred following component by its ratio of weight and number is: get corn cob 100 weight part, nitric acid 80 weight part, sulfuric acid 50 weight part, pentanoic 5 weight part, camphor 5 weight part, soda ash 3 weight part, alcohol 90 weight part.
Be equipped with standby 100 weight part vegetable fibres, preferential component and ratio of weight and number are: get corn stalk 50 weight part, bamboo wood 50 weight part, nitric acid 40 weight part, sulfuric acid 10 weight part, pentanoic 1 weight part, camphor 1 weight part, soda ash 9 weight part, lacquer thinner 55 weight part.
Be equipped with standby 100 weight part vegetable fibres, preferential component and ratio of weight and number are: get corn cob 60 weight part, sugarcane waste residue 40 weight part, nitric acid 65 weight part, sulfuric acid 26 weight part, pentanoic 2 weight part, camphor 2 weight part, soda ash 6 weight part, ether 80 weight part.
Be equipped with standby 100 weight part vegetable fibres, preferential component and ratio of weight and number are: get bamboo wood 40 weight part, waste of flax 20 weight part, reed 30 weight part, nitric acid 60 weight part, sulfuric acid 30 weight part, pentanoic 1.5 weight part, camphor 1.5 weight part, soda ash 5 weight part, acetone 70 weight part.
Smokeless Mierocrystalline cellulose preparation method of the present invention comprises following step and gathers:
The various vegetable fibre Powder screen choosings of pulverizing are classified as one-level 120 order, secondary 60-100 order by 1. raw material screening classification;
2. soak respectively with soda ash, the soda ash of the adaptive weight part in 600 weight parts and above-mentioned preferred component of adding water by the vegetable fibre of 100 weight parts, soak at room temperature 72 hours after stirring, by soak mainly impurity elimination, grease removal, except starch;
3. clear water washing, dry, by above-mentioned immersion impurity elimination, grease removal, except the plant after starch one after another with clear water washing to do not have alkalescence neutrals, adopt test paper test, then dried by the vegetable fibre of rinsing, water content can be within 10%;
4. nitration reaction, with vegetable fibre 100 weight part after drying, adds nitric acid by ratio of weight and the number of copies and sulfuric acid mix acid liquor, and put into reactor and stir, temperature that the temperature remains within the normal range, reacts 1 hour, generates itrated compound vegetable fibre;
5. rinsing, carries out rinsing by the vegetable fibre of nitration reaction, disacidify, impurity elimination, at least rinsing four times, with test paper test to complete neutral standard;
6. centrifugal drying of drying, the itrated compound vegetable fibre after rinsing carries out centrifugal drying, and adopt steam drying, 30 minutes to 2 hours time, vapor temperature is 60 °-150 °, makes water content in itrated compound plant cellulose lower than 2%;
7. add stablizer preparation to pulverize, 0.5-5 weight part pentanoic and 0.5-5 weight part camphor is added again in the centrifugal dried itrated compound vegetable fibre that dries, and after being atomized into mixture by dissolution with solvents by ratio of weight and the number of copies, mix, be ground into 120 orders and namely obtain the quick-fried medicament of described smokeless Mierocrystalline cellulose firworks string.
The advantage that the present invention has and positively effect are:
1, owing to adopting the plant cellulose through nitration treatment to be fireworks medicament, smog can not be produced during preparation firework powder afterfire, efficiently solve the difficult problem that when traditional firworks string detonation is put, cigarette is large, cigarette is dense, the present invention is chloracid potassium not, the product of not chloride hydrochlorate composition, so safety performance is high, preparation firework product production, transport and storage and set off shock general in process and friction can not be exploded and had an accident.
2, friction sensitivity is less than 60%, actual measurement 6-34%; Impact sensitivity is less than 50%, actual measurement 30-40%; Rate of moisture absorption is low, is less than 2%, and actual measurement 1.2-1.4%, is all better than national standard, and therefore substantially increase the security that firework product is produced and seted off, its agent stability is good, makes firework product not moisture-sensitive, improves the quality of the quick-fried product of firworks string.
3, be main raw material because the present invention is corn cob, corn stalk, waste of flax, Pericarppium arachidis hypogaeae, sugarcane waste residue, reed and the bamboo wood adopting farm crop to abandon, therefore raw material sources are extensive, inexpensive, can reduce firework product cost 20-30%; Make the plant resources discarded be able to regeneration simultaneously, for making full use of of rural resource opens new approach, add huge Social and economic benef@.
4, smokeless, tasteless, nontoxic, dustless dye when the firework product of the present invention's preparation is seted off, meet environment protection requirement, improve the visual effect of firework display simultaneously, make the pattern modelling setting off product more clear, gorgeous colorful, the preparation being applicable to various fireworks series product is produced, as various display shell, combined firework, cold light firework, subtitling firework, toy firework, Fireworks on water etc.; Can to set off or indoor are seted off outdoor; Its medicament can be processed as micro-mealy medicine according to the preparation needs of firework product medicine or be microgranular medicament or sheet medicament, so smokeless cellulose portion of the present invention is simple, easy to prepare, cost is low.
The present invention as the quick-fried with medicament of firworks string through national fireworks and firecrackers product quality supervision and inspection center and fireworks and firecrackers quality supervision and test test center of Ministry of Agriculture detected result respectively in table 1, table 2:
Table 1: the quick-fried Safety Inspection report of national fireworks and firecrackers product quality supervision and inspection center firworks string.
Inspection numbering: WA20122336 client or individual: Pan little Qiu
Table 2: the quick-fried Safety Inspection report of fireworks and firecrackers quality supervision and test test center of Ministry of Agriculture firworks string.
Inspection numbering: №: 2012-15-220 client or individual: Pan little Qiu
Embodiment:
Below in conjunction with specific embodiment, the present invention is described in further detail.
Smokeless Mierocrystalline cellulose of the present invention, quick-fried for preparing firworks string, be solid-state micro mist shape or microgranular medicament, it is characterized in that, it is made through nitration reaction by vegetable fibre, and its component and ratio of weight and number are:
Vegetable fibre: refer to the corn cob through pulverizing, corn stalk, bamboo wood, waste of flax, Pericarppium arachidis hypogaeae, reed, sugarcane waste residue, wherein any one or multiple any ratio of weight and number mixture, consumption is 100 weight parts;
Nitrating agent: described nitrating agent is nitric acid and sulfuric acid mixture, wherein concentration of nitric acid is 60-98%, and consumption is 40-80 weight part, and sulfuric acid concentration is 60-98%, and consumption is 10-50 weight part;
Stablizer: described stablizer is the mixture of pentanoic and camphor, consumption is pentanoic 0.5-5 weight part, camphor 0.5-5 weight part.
Soda ash: consumption is 1-10 weight part;
Solvent: the wherein one of alcohol or lacquer thinner or ether or acetone, consumption is 50-100 weight part.
Embodiment 1
Be equipped with standby 100 weight part vegetable fibres, preferred following component by its ratio of weight and number is: get corn cob 100 weight part, nitric acid 80 weight part, sulfuric acid 50 weight part, pentanoic 5 weight part, camphor 5 weight part, soda ash 3 weight part, alcohol 90 weight part.
Smokeless Mierocrystalline cellulose preparation method of the present invention comprises following step and gathers:
The various vegetable fibre Powder screen choosings of pulverizing are classified as one-level 120 order, secondary 60-100 order by 1. raw material screening classification;
2. soak respectively with soda ash, the soda ash of the adaptive weight part in 600 weight parts and above-mentioned preferred component of adding water by the vegetable fibre of 100 weight parts, soak at room temperature 72 hours after stirring, by soak mainly impurity elimination, grease removal, except starch;
3. clear water washing, dry, by above-mentioned immersion impurity elimination, grease removal, except the plant after starch one after another with clear water washing to do not have alkalescence neutrals, adopt test paper test, then dried by the vegetable fibre of rinsing, water content can be within 10%;
4. nitration reaction, with vegetable fibre 100 weight part after drying, adds the nitric acid of 40-80 weight part and the sulfuric acid mix acid liquor of 10-50 weight part, and put into reactor and stir, temperature that the temperature remains within the normal range, reacts 1 hour, generates itrated compound vegetable fibre;
5. rinsing, carries out rinsing by the vegetable fibre of nitration reaction, disacidify, impurity elimination, at least rinsing four times, with test paper test to complete neutral standard;
6. centrifugal drying of drying, the itrated compound vegetable fibre after rinsing carries out centrifugal drying, seasoning, makes water content in itrated compound plant cellulose lower than 2%;
7. add stablizer preparation to pulverize, 0.5-5 weight part pentanoic and 0.5-5 weight part camphor is added again in the centrifugal dried itrated compound vegetable fibre that dries, and after being atomized into mixture by dissolution with solvents by ratio of weight and the number of copies, mix, be ground into 120 orders and namely obtain the quick-fried medicament of described smokeless Mierocrystalline cellulose firworks string.
Embodiment 2
Be equipped with standby 100 weight part vegetable fibres, preferred following component by its ratio of weight and number is: get corn stalk 50 weight part, bamboo wood 50 weight part, nitric acid 40 weight part, sulfuric acid 10 weight part, pentanoic 1 weight part, camphor 1 weight part, soda ash 9 weight part, lacquer thinner 55 weight part, obtains the quick-fried medicament of smokeless Mierocrystalline cellulose firworks string of the present invention by the preparation method identical with embodiment 1.
Embodiment 3
Be equipped with standby 100 weight part vegetable fibres, preferred following component by its ratio of weight and number is: get corn cob 50 weight part, Pericarppium arachidis hypogaeae 30 weight part, sugarcane waste residue 20 weight part, nitric acid 65 weight part, sulfuric acid 26 weight part, pentanoic 2 weight part, camphor 2 weight part, soda ash 6 weight part, ether 80 weight part, obtains the quick-fried medicament of smokeless Mierocrystalline cellulose firworks string of the present invention by the preparation method identical with embodiment 1.
Embodiment 4
Be equipped with standby 100 weight part vegetable fibres, preferred following component by its ratio of weight and number is: get bamboo wood 40 weight part, waste of flax 20 weight part, reed 30 weight part, nitric acid 60 weight part, sulfuric acid 30 weight part, pentanoic 1.5 weight part, camphor 1.5 weight part, soda ash 5 weight part, acetone 70 weight part, obtains the quick-fried medicament of smokeless Mierocrystalline cellulose firworks string of the present invention by the preparation method identical with embodiment 1.
Claims (5)
1. a smokeless Mierocrystalline cellulose, quick-fried for preparing firworks string, be solid-state micro mist shape or microgranular medicament, it is characterized in that, it is made through nitration reaction by vegetable fibre, and its component and ratio of weight and number are:
Vegetable fibre: refer to the corn cob through pulverizing, corn stalk, bamboo wood, waste of flax, Pericarppium arachidis hypogaeae, reed, sugarcane waste residue, wherein any one or multiple any ratio of weight and number mixture, consumption is 100 weight parts;
Nitrating agent: described nitrating agent is nitric acid and sulfuric acid mixture, wherein concentration of nitric acid is 60-98%, and consumption is 40-80 weight part, and sulfuric acid concentration is 60-98%, and consumption is 10-50 weight part;
Stablizer: described stablizer is the mixture of pentanoic and camphor, consumption is pentanoic 0.5-5 weight part, camphor 0.5-5 weight part;
Soda ash: consumption is 1-10 weight part;
Solvent: the wherein one of alcohol or lacquer thinner or ether or acetone, consumption is 50-100 weight part;
Described smokeless cellulosic preparation method comprises the following steps:
The various vegetable fibre Powder screen choosings of pulverizing are classified as one-level 120 order, secondary 60-100 order by 1. raw material screening classification;
2. soak respectively with soda ash, the soda ash of add water by the vegetable fibre of 100 weight parts 600 weight parts and 1-10 weight part, soak at room temperature 72 hours after stirring, by soak mainly impurity elimination, grease removal, except starch;
3. clear water washing, drying, by above-mentioned immersion impurity elimination, grease removal, except the vegetable fibre clear water washing after starch is to the neutrals not having alkalescence, adopt test paper test, then dried by the vegetable fibre of rinsing, water content can be within 10%;
4. nitration reaction, with vegetable fibre 100 weight part after drying, adds nitric acid by ratio of weight and the number of copies and sulfuric acid mix acid liquor, and put into reactor and stir, temperature that the temperature remains within the normal range, reacts 1 hour, generates itrated compound vegetable fibre;
5. rinsing, carries out rinsing by the vegetable fibre of nitration reaction, disacidify, impurity elimination, at least rinsing four times, with test paper test to complete neutral standard;
6. centrifugal drying of drying, the itrated compound vegetable fibre after rinsing carries out centrifugal drying, and adopt steam drying, 30 minutes to 2 hours time, vapor temperature is 60 DEG C-150 DEG C, makes water content in itrated compound plant cellulose lower than 2%;
7. add stablizer preparation to pulverize, 0.5-5 weight part pentanoic and 0.5-5 weight part camphor is added again in the centrifugal dried itrated compound vegetable fibre that dries, and after being atomized into mixture by dissolution with solvents by ratio of weight and the number of copies, mix, be ground into 120 orders.
2. smokeless Mierocrystalline cellulose according to claim 1, it is characterized in that, its component and ratio of weight and number are: be equipped with standby 100 weight part vegetable fibres, get corn cob 100 weight part, nitric acid 80 weight part, sulfuric acid 50 weight part, pentanoic 5 weight part, camphor 5 weight part, soda ash 3 weight part, alcohol 90 weight part.
3. smokeless Mierocrystalline cellulose according to claim 1, it is characterized in that, its component and ratio of weight and number are: be equipped with standby 100 weight part vegetable fibres, get corn stalk 50 weight part, bamboo wood 50 weight part, nitric acid 40 weight part, sulfuric acid 10 weight part, pentanoic 1 weight part, camphor 1 weight part, soda ash 9 weight part, lacquer thinner 55 weight part.
4. smokeless Mierocrystalline cellulose according to claim 1, it is characterized in that, its component and ratio of weight and number are: be equipped with standby 100 weight part vegetable fibres, get corn cob 50 weight part, sugarcane waste residue 20 weight part, Pericarppium arachidis hypogaeae 30 weight part, nitric acid 65 weight part, sulfuric acid 26 weight part, pentanoic 2 weight part, camphor 2 weight part, soda ash 6 weight part, ether 80 weight part.
5. smokeless Mierocrystalline cellulose according to claim 1, it is characterized in that, its component and ratio of weight and number are: be equipped with standby 100 weight part vegetable fibres, get bamboo wood 40 weight part, waste of flax 20 weight part, reed 30 weight part, nitric acid 60 weight part, sulfuric acid 30 weight part, pentanoic 1.5 weight part, camphor 1.5 weight part, soda ash 5 weight part, acetone 70 weight part.
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| CN109764762B (en) * | 2019-03-07 | 2021-05-28 | 浏阳东顺花炮新材料技术开发有限公司 | Continuous production system of tobacco peanut powder |
| CN111056884B (en) * | 2019-11-27 | 2023-04-25 | 江西吉润花炮新材料科技有限公司 | Safe, smokeless and sulfur-free dampproof agent and preparation method thereof |
| CN111533629A (en) * | 2020-05-27 | 2020-08-14 | 湖南坤普科技有限公司 | Firework and firecracker containing nitrocellulose and method for improving burning speed of firework and firecracker |
| CN111848823A (en) * | 2020-08-18 | 2020-10-30 | 潘小秋 | Ester alcohol bamboo wood cellulose and preparation method thereof |
| CN116497465A (en) * | 2023-05-17 | 2023-07-28 | 中应国强安全科技(北京)有限公司 | Amaranth plant fiber, preparation method thereof and firework |
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Address after: 410300, Huai River Street office, Hunan, Liuyang Province, refers to the back road 50 Applicant after: Pan Xiaoqiu Address before: 410300, Hunan, Liuyang, refers to the back of the arch, No. 022, Beiqiao Applicant before: Pan Xiaoqiu |
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Effective date of registration: 20210918 Address after: 410300 No. 49, Shishuang Road, Jili street, Liuyang City, Changsha City, Hunan Province Patentee after: Hunan Xusheng New Material Technology Co.,Ltd. Address before: 410300 huaichuan sub district office, Liuyang City, Hunan Province, No. 50 zhibeichong Road Patentee before: Pan Xiaoqiu |
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Effective date of registration: 20220831 Address after: Dasheng Village, Chengtanjiang Town, Liuyang City, Changsha City, Hunan Province 410300 Patentee after: Liuyang Huajin Fireworks Manufacturing Co.,Ltd. Address before: 410300 No. 49, Shishuang Road, Jili street, Liuyang City, Changsha City, Hunan Province Patentee before: Hunan Xusheng New Material Technology Co.,Ltd. |
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