CN101343329A - Multi-hydroxyalkyl cellulose ether nitrate and preparation thereof - Google Patents
Multi-hydroxyalkyl cellulose ether nitrate and preparation thereof Download PDFInfo
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- CN101343329A CN101343329A CNA2008101178186A CN200810117818A CN101343329A CN 101343329 A CN101343329 A CN 101343329A CN A2008101178186 A CNA2008101178186 A CN A2008101178186A CN 200810117818 A CN200810117818 A CN 200810117818A CN 101343329 A CN101343329 A CN 101343329A
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Abstract
The invention relates to a variety of hydroxyalkyl cellulose ether nitrate and the preparation method, which belongs to the technical field of the high polymer chemistry. The invention adopts the modified product of cellulose, namely the hydroxyalkyl cellulose ether to react in a nitrification system composed of fuming nitric acid HNO3 and organic solvent CH2Cl2 under the temperature range of 15 DEG C to 30 DEG C and under the agitation for 25 minutes to 40 minutes, and the hydroxyalkyl cellulose ether nitrate with the nitrogen content within a certain range is obtained through the processes of settling out, washing, stability handling (washing through boiling) in water. The variety of hydroxyalkyl cellulose ether nitrate and the preparation method have the advantages that methylene dichloride is adopted as dispersant, thereby having higher nitration efficiency, the synthesis process and the product stability handling are simple, the nitration product of the high nitrogen content cellulose ether with higher purity and stability can be obtained and is novel thermoplastic energetic adhesive and can be applied to various fields of gunpowder, explosive, film negative, coating material, spray painting, plastic and film forming material manufactures according to differences of the substitution degree of the cellulose ether and the nitrogen content of the nitration product.
Description
Technical field
The present invention relates to class hydroxyalkyl cellulose ether nitrate and preparation method thereof, particularly heterogeneous method prepares the method for multiple hydroxyalkyl cellulose ether nitrate, belongs to technical field of polymer chemistry.
Background technology
Mierocrystalline cellulose is a kind of natural macromolecular material of wide material sources, and the ether of cellulose that obtains after chemical modification is cellulosic derivative.Hydroxyalkyl cellulose ether is the ether of cellulose that has hydroxyl-OH on the class side chain, as hydroxyethyl ether cellulose HEC, hydroxypropylcelluloether ether HPC, dihydroxypropyl ether of cellulose GEC etc., these-have on the glucose cyclic group (AGU) of OH and cellulose macromolecule-OH is the same to have big actively, can both generate nitric ether with nitric acid generation esterification.Because the intramolecularly plastification has been played in the access of hydroxyalkyl side chain, has reduced the regularity of cellulose macromolecule chain, its degree of crystallinity is descended, second-order transition temperature reduces, and kindliness improves.Therefore, through the cellulose ether nitrate that obtains after the nitration reaction, be that a class has thermoplastic energetic material, can be used as the tackiness agent of solid propellant.The molar substitution MS of ether of cellulose is influential to the thermoplasticity of its nitration product, the hydroxyalkyl cellulose ether nitrate of different etherificate substitution value MS and degree of nitrification has different purposes, can be used in industry and makes gunpowder, explosive, film, coating, sprays paint, fields such as plastics and film forming material.
Also there is not patent report about hydroxyalkyl cellulose ether nitrate and nitrated technology thereof at present.But existing more than 100 year of cellulosic nitrated technical study has successively been invented the nitric acid vapor esterification process, nitric acid esterification process, nitric acid-sulfuric acid nitration mixture esterification process, nitric acid-phosphorus nitration mixture esterification process, nitric acid-acetic acid esterification process and inert media and nitration mixture esterification process.In these methods, having only the nitrated technology of nitric-sulfuric acid to realize industrialization, is the main method of producing nitro-cotton (NC) at present.Twentieth century fritz's thirties Thinins and Weihe have invented a kind of nitrated technology of industrial Mierocrystalline cellulose that is used for, promptly anhydrous nitric acid is dissolved in the organic solvent, this solvent not with nitric acid reaction, do not dissolve soluble cotton NC yet, after isolating product, through stable treatment, the NC that obtains has higher purity and secular stability.Units such as Russia noise made in coughing or vomiting mountain chemical research institute have carried out a large amount of research to the Mierocrystalline cellulose esterification under the situation of methylene dichloride existence, change esterifying agent and form the soluble cotton that obtains different content.
Summary of the invention
The purpose of this invention is to provide a class hydroxyalkyl cellulose ether nitrate and a synthetic method thereof.
Product general formula of the present invention is: [(C
6H
7O
2) (OH)
x(ONO
2)
y(-OR)
(3-x-y)]
nWherein: x, y satisfies 0＜x＜3,0＜y＜3 and 0＜(x+y)＜3;
R representative-CH
2CH
2-OR ' ,-CH
2CH (OR ') CH
3Or-CH
2CH (OR ') CHOR ';
R ' representative-H or-NO
2
The synthetic method of a class hydroxyalkyl cellulose ether nitrate of the present invention, chemical equation is:
Its concrete preparation process is:
The preparation of step 1, reaction solution: under the normal temperature, nitrosonitric acid joined in the analytically pure methylene dichloride to stir make nitration reaction liquid, wherein the scope of the shared nitration reaction liquid of nitrosonitric acid mass percent is 20%～70%.
Step 2, with ether of cellulose dry to moisture content less than 5%, put into pulverizer then and pulverize, size range is 60 orders～200 orders.
Step 3, the reaction solution in the step 1 is joined in the nitrator, stir, stir speed (S.S.) is 200 rev/mins～300 rev/mins, ether of cellulose in the step 2 is added in the nitration reaction liquid, the reinforced time is controlled within the 10min, 15 ℃～30 ℃ of range of reaction temperature continue stirring reaction 25min～40min, obtain containing the mixed solution of methylene dichloride, nitric acid and target product; Wherein, the mass ratio 40～60: 1 of nitration reaction liquid and ether of cellulose, ether of cellulose are any one or the arbitrary combination between them of hydroxyethyl ether cellulose, hydroxypropylcelluloether ether and dihydroxypropyl ether of cellulose.
Step 4, above-mentioned mixed solution poured in the water stir, suction filtration obtains white precipitate.
Step 5, above-mentioned white precipitate is washed with water and suction filtration at normal temperatures, obtain preliminary target product.
Step 6, above-mentioned preliminary target product poured into to boil under the normal pressure in the boiling water wash 30min～60min, cooling back suction filtration is washed with water at normal temperatures when the pH value reaches neutrality again and carries out suction filtration, promptly obtains target product.
Beneficial effect:
1) this synthetic method is simple, saves time product purity height, Heat stability is good.
2) three kinds of hydroxyalkyl cellulose ether nitrates of synthetic of the present invention are that the novel thermoplasticity of a class contains can tackiness agent, and to compare second-order transition temperature low with the soluble cotton of identical nitrogen content.According to the molar substitution of ether of cellulose and the difference of nitration product nitrogen content thereof, different field such as the cellulose ether nitrate that makes can be applied in and make gunpowder, explosive, film, coating, spray paint, plastics and film forming material.
Description of drawings
The hydroxyalkyl cellulose ether nitrate preparation were established
Specific embodiment
Embodiment 1
The preparation of reaction solution: under the normal temperature, the 50g nitrosonitric acid joined in the analytically pure methylene dichloride of 200g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 0.5 dihydroxypropyl ether of cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
The dihydroxypropyl ether of cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.58 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 12.6%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 375K.
Embodiment 2
The preparation of reaction solution: under the normal temperature, the 125g nitrosonitric acid joined in the analytically pure methylene dichloride of 125g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 0.5 dihydroxypropyl ether of cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
The dihydroxypropyl ether of cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.65 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 13.6%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 379K.
Embodiment 3
The preparation of reaction solution: under the normal temperature, the 175g nitrosonitric acid joined in the analytically pure methylene dichloride of 75g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 0.5 dihydroxypropyl ether of cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
The dihydroxypropyl ether of cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.56 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 12.5%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 368K.
Embodiment 4
The preparation of reaction solution: under the normal temperature, the 100g nitrosonitric acid joined in the analytically pure methylene dichloride of 150g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 1.0 dihydroxypropyl ether of cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
The dihydroxypropyl ether of cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.64 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 13.28%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 365K.
Embodiment 5
The preparation of reaction solution: under the normal temperature, the 125g nitrosonitric acid joined in the analytically pure methylene dichloride of 125g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 1.0 dihydroxypropyl ether of cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
The dihydroxypropyl ether of cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.54 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 12.8%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 361K.
Embodiment 6
The preparation of reaction solution: under the normal temperature, the 150g nitrosonitric acid joined in the analytically pure methylene dichloride of 100g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 0.5 dihydroxypropyl ether of cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
The dihydroxypropyl ether of cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.60 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 12.9%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 385K.
Embodiment 7
The preparation of reaction solution: under the normal temperature, the 125g nitrosonitric acid joined in the analytically pure methylene dichloride of 125g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 1.6 hydroxyethyl ether cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
Hydroxyethyl ether cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.20 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 10.5%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 344K.
Embodiment 8
The preparation of reaction solution: under the normal temperature, the 100g nitrosonitric acid joined in the analytically pure methylene dichloride of 100g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 2.5 hydroxyethyl ether cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
Hydroxyethyl ether cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.16 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 8.1%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 326K.
Embodiment 9
The preparation of reaction solution: under the normal temperature, the 125g nitrosonitric acid joined in the analytically pure methylene dichloride of 125g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 2.0 hydroxyethyl ether cellulose, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
Hydroxyethyl ether cellulose is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.15 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 7.99%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 333K.
Embodiment 10
The preparation of reaction solution: under the normal temperature, the 100g nitrosonitric acid joined in the analytically pure methylene dichloride of 150g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 0.5 hydroxypropylcelluloether ether, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
Hydroxypropylcelluloether ether is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.61 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 13.0%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 391K.
Embodiment 11
The preparation of reaction solution: under the normal temperature, the 150g nitrosonitric acid joined in the analytically pure methylene dichloride of 100g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 0.3 hydroxypropylcelluloether ether, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
Hydroxypropylcelluloether ether is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.67 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 13.4%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 403K.
Embodiment 12
The preparation of reaction solution: under the normal temperature, the 125g nitrosonitric acid joined in the analytically pure methylene dichloride of 125g to stir make nitration reaction liquid.
Take by weighing the 5g molar substitution and be 4.0 hydroxypropylcelluloether ether, dry to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
Hydroxypropylcelluloether ether is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.2 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 7.8%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 332K.
Embodiment 13
The preparation of reaction solution: under the normal temperature, the 125g nitrosonitric acid joined in the analytically pure methylene dichloride of 125g to stir make nitration reaction liquid.
Take by weighing the 2.5g molar substitution and be 4.0 hydroxypropylcelluloether ether and 2.5g molar substitution and be 0.3 dihydroxypropyl ether of cellulose, dry behind the uniform mixing to moisture content 3%, put into pulverizer then and pulverize, size range is 80 orders.
The mixed cellulose ethers that crushes is joined in the reaction solution, and the reinforced time is 3min, and temperature is 22 ℃, and reaction 30min stops to stir.
Reaction mixture is poured in the container of 800ml water and stirred precipitating, suction filtration gets white depositions behind the 10min.With this throw out restir washing 2 times, use 500ml water, washing 10min at every turn.Behind the suction filtration, product boils in the 500ml boiling water and washes 30min, cooling back suction filtration.And then, wash 10min with 500ml normal-temperature water washing 2 times at every turn, and record the pH value for neutral, obtain this product behind the suction filtration.
Its performance index are:
Quality after the products obtained therefrom oven dry is 1.25 times of the ether of cellulose quality that adds.Nitrogen content wt (N) % that the element method records product is 10.5%.The exsiccant product is dissolved in acetone makes 4% solution, and, carry out dynamic properties test (DMA method) then, its second-order transition temperature T by curtain coating legal system film
gBe 352K.
Claims (3)
1, a class hydroxyalkyl cellulose ether nitrate is characterized in that:
General formula is: [(C
6H
7O
2) (OH)
x(ONO
2)
y(-OR)
(3-x-y)]
n
Wherein: x, y satisfies 0＜x＜3,0＜y＜3 and 0＜(x+y)＜3;
R is-CH
2CH
2-OR ' ,-CH
2CH (OR ') CH
3Or-CH
2CH (OR ') CHOR ';
R ' is-H or-NO
2
2, the preparation method of a class hydroxyalkyl cellulose ether nitrate is characterized in that preparation process is as follows:
The preparation of step 1, reaction solution: under the normal temperature, nitrosonitric acid joined in the analytically pure methylene dichloride to stir make nitration reaction liquid, wherein the scope of the shared nitration reaction liquid of nitrosonitric acid mass percent is 20%～70%;
Step 2, with ether of cellulose dry to moisture content less than 5%, put into pulverizer then and pulverize, size range is 60 orders～200 orders;
Step 3, the reaction solution in the step 1 is joined in the nitrator, stir, stir speed (S.S.) is 200 rev/mins～300 rev/mins, ether of cellulose in the step 2 is added in the nitration reaction liquid, the reinforced time is controlled within the 10min, 15 ℃～30 ℃ of range of reaction temperature continue stirring reaction 25min～40min, obtain containing the mixed solution of methylene dichloride, nitric acid and target product; Wherein, the mass ratio 40～60: 1 of nitration reaction liquid and ether of cellulose, ether of cellulose are any one or the arbitrary combination between them of hydroxyethyl ether cellulose, hydroxypropylcelluloether ether and dihydroxypropyl ether of cellulose;
Step 4, above-mentioned mixed solution poured in the water stir, suction filtration obtains white precipitate;
Step 5, above-mentioned white precipitate is washed with water and suction filtration at normal temperatures, obtain preliminary target product;
Step 6, above-mentioned preliminary target product poured into to boil under the normal pressure in the boiling water wash 30min～60min, cooling back suction filtration is washed with water at normal temperatures when the pH value reaches neutrality again and carries out suction filtration, promptly obtains target product.
3, the preparation method of a class hydroxyalkyl cellulose ether nitrate as claimed in claim 2 is characterized in that: ether of cellulose is any one or the arbitrary combination between them of hydroxyethyl ether cellulose, hydroxypropylcelluloether ether and dihydroxypropyl ether of cellulose.
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|---|---|---|---|
| CNA2008101178186A CN101343329A (en) | 2008-08-04 | 2008-08-04 | Multi-hydroxyalkyl cellulose ether nitrate and preparation thereof |
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|---|---|---|---|
| CNA2008101178186A CN101343329A (en) | 2008-08-04 | 2008-08-04 | Multi-hydroxyalkyl cellulose ether nitrate and preparation thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351955A (en) * | 2011-08-05 | 2012-02-15 | 四川北方硝化棉股份有限公司 | Nitrocotton boiling and washing method |
| CN102811980A (en) * | 2010-01-19 | 2012-12-05 | 克里尔斯巴克有限责任公司 | Method for preparing a pyrotechnic composition and charge |
| CN107151271A (en) * | 2017-06-05 | 2017-09-12 | 常熟理工学院 | A kind of preparation method of the low quick-fried temperature nitrocotton of high energy |
| CN109369811A (en) * | 2018-09-19 | 2019-02-22 | 南通泰利达化工有限公司 | A kind of optimization process preparing carboxymethyl cellulose nitrate |
-
2008
- 2008-08-04 CN CNA2008101178186A patent/CN101343329A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102811980A (en) * | 2010-01-19 | 2012-12-05 | 克里尔斯巴克有限责任公司 | Method for preparing a pyrotechnic composition and charge |
| CN102811980B (en) * | 2010-01-19 | 2016-05-11 | 克里尔斯巴克有限责任公司 | For the preparation of the method for pyrotechnic composition and powder charge |
| CN102351955A (en) * | 2011-08-05 | 2012-02-15 | 四川北方硝化棉股份有限公司 | Nitrocotton boiling and washing method |
| CN107151271A (en) * | 2017-06-05 | 2017-09-12 | 常熟理工学院 | A kind of preparation method of the low quick-fried temperature nitrocotton of high energy |
| CN107151271B (en) * | 2017-06-05 | 2019-06-25 | 常熟理工学院 | A kind of preparation method of the low quick-fried temperature nitrocotton of high energy |
| CN109369811A (en) * | 2018-09-19 | 2019-02-22 | 南通泰利达化工有限公司 | A kind of optimization process preparing carboxymethyl cellulose nitrate |
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