CN102180978A - Technology for producing substitution-degree hydroxyethyl cellulose - Google Patents
Technology for producing substitution-degree hydroxyethyl cellulose Download PDFInfo
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Abstract
The invention discloses a technology for producing substitution-degree hydroxyethyl cellulose, relating to the field of fine chemical industry. A multistep method, namely the addition of ethylene oxide according to substitution-degree requirement for multiple times, is adopted, wherein the concentration of ethylene oxide in a system is stabilized in a certain range; side-reaction speed is controlled at a low state and beneficial to the stable proceeding of positive reaction; the substitution degree can achieve 2.0-2.6; simultaneously, the uniformity degree of molecular substitution can be improved greatly, the quality stability of products is enhanced, the fungus resistance of the products can be improved by 30% and the shelf life of produced emulsion paint is prolonged by three months; and the whole reaction process of the technology for producing the substitution-degree hydroxyethyl cellulose is controlled by a computer DCS (Distribution Control System) program, the labor intensity is lowered, a production device of the same scale can save twelve fixed members, and the labor efficiency and the production safety are improved.
Description
Technical field
The present invention relates to field of fine chemical, specifically a kind of technology of producing the high substitution value Natvosol.
Background technology
Natvosol be with natural cellulose under the effect of solvent and alkali and reacting ethylene oxide and making, at present domestic whole one step of employings etherification technologies, the oxyethane of promptly disposable adding capacity, segmentation is reacted and is made then; Because oxyethane excessive, high density is in system, side reaction is very fast, be not easy control, substitution value generally can only reach 1.5-2.0, influence the effect of this product in emulsion paint, so the present domestic emulsion paint production unit that possesses scale has the Natvosol of 80% employing import.
Summary of the invention
For solving the technical problem of above-mentioned existence, the invention provides a kind of technology of producing the high substitution value Natvosol, require to add oxyethane several times according to substitution value, to carry out the substep etherificate and make, entire reaction course is controlled by computer program.
For achieving the above object, the technical solution used in the present invention is as follows:
Realize by following steps:
(1) pulverizes: the refined cellulose process of 1000 mass fractions is pulverized, separated dedusting;
(2) alkalization: the alcoholic solution and the stirring that in reactor, add the 5000-12000 mass fraction, the sheet alkali that adds the 200-280 mass fraction, be warmed up to 60-85 ℃ of choline, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 0.5-1.5 hour down at 15-35 ℃;
(3) reaction: be divided into for two steps,
The oxyethane that at first in reactor, adds formula ratio 40%-65%, this step reaction divides two stages, fs is to be reaction 0.5-1.5 hour under 45-60 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 0.5-1.5 hour under 65-85 ℃ the situation in temperature of reaction;
The oxyethane that in reactor, adds formula ratio 35%-60% then again, this step reaction divides two stages, fs is to be reaction 0.5-1.5 hour under 45-60 ℃ the situation in temperature of reaction, and subordinate phase is to be 0.5-2 hour following reaction times of situation of 65-85 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the acid solution that adopts the 300-500 mass fraction is under 40-60 ℃ the situation neutralization reaction 0.5-1 hour in temperature, with the pH value of adjusting gained solution between 5.5-8.5;
(5) flash liberation: separate making solid materials enter the washing still, liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1-2 hour under temperature 20-35 ℃ situation in the washing still;
(7) secondary separation: the solid-liquid separation in the washing still, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
(1) pulverizes: the refined cellulose process of 1000 mass fractions is pulverized, separated dedusting;
(2) alkalization: the alcoholic solution and the stirring that in reactor, add the 6000-10000 mass fraction, the sheet alkali that adds the 220-250 mass fraction, be warmed up to 70-75 ℃ of choline, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 0.5-1 hour down at 20-30 ℃;
(3) reaction: be divided into for two steps,
The oxyethane that at first in reactor, adds formula ratio 40%-65%, this step reaction divides two stages, fs is to be reaction 0.5-1 hour under 50-55 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 0.5-1 hour under 70-75 ℃ the situation in temperature of reaction;
The oxyethane that in reactor, adds formula ratio 35%-60% then again, this step reaction divides two stages, fs is to be reaction 0.5-1 hour under 50-55 ℃ the situation in temperature of reaction, and subordinate phase is to be 0.5-1 hour following reaction times of situation of 70-75 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the acid solution that adopts the 350-450 mass fraction is under 40-60 ℃ the situation neutralization reaction 0.5-1 hour in temperature, with the pH value of adjusting gained solution between 5.5-8.5;
(5) flash liberation: separate making solid materials enter the washing still, liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1-2 hour under temperature 20-35 ℃ situation in the washing still;
(7) secondary separation: the solid-liquid separation in the washing still, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
The present invention adopts multistep processes---promptly require to add several times oxyethane according to substitution value, the concentration stabilize of oxyethane in system within the specific limits, the side reaction speed control is at low state, help steadily carrying out of positive reaction, substitution value can reach 2.0-2.6, can improve simultaneously the degree of uniformity that polymer replaces greatly, improve product quality stability, the midew proof of its product can improve 30%, the emulsion paint shelf life extension of producing 3 months, entire reaction course of the present invention adopt computer DCS time variable control, have reduced labour intensity, equal scale production device can be saved 12 staffings, raises labour efficiency and production security.
Description of drawings
Accompanying drawing is a schematic flow sheet of the present invention.
Embodiment
Describe the present invention below in conjunction with the drawings and specific embodiments:
Embodiment 1
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: in reactor, add the aqueous isopropanol and the stirring of 5000 mass fractions, add the sheet alkali of 200 mass fractions, be warmed up to 60 ℃ of cholines, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 0.5 hour down at 20 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 40% in reactor, this step reaction divides two stages, and the fs is to be reaction 1.5 hours under 45 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 1 hour under 75 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 60% again in reactor, this step reaction divides two stages, and the fs is to be reaction 1 hour under 55 ℃ the situation in temperature of reaction, and subordinate phase is to be 0.5 hour following reaction times of situation of 85 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the acetum that adopts 300 mass fractions is neutralization reaction 0.5 hour under 40 ℃ the situation in temperature, is 5.5 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 2 hours under the situation of 20 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 2
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: in reactor, add the n-propyl alcohol solution and the stirring of 12000 mass fractions, add the sheet alkali of 280 mass fractions, be warmed up to 70 ℃ of cholines, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 1.5 hours down at 15 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 65% in reactor, this step reaction divides two stages, and the fs is to be reaction 0.5 hour under 60 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 0.5 hour under 85 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 35% again in reactor, this step reaction divides two stages, and the fs is to be reaction 0.5 hour under 60 ℃ the situation in temperature of reaction, and subordinate phase is to be 2 hours following reaction times of situation of 65 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the hydrochloric acid soln that adopts 500 mass fractions is neutralization reaction 1 hour under 50 ℃ the situation in temperature, is 7 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1 hour under the situation of 35 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 3
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: in reactor, add the butanol solution and the stirring of 10000 mass fractions, add the sheet alkali of 250 mass fractions, be warmed up to 85 ℃ of cholines, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 1 hour down at 35 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 50% in reactor, this step reaction divides two stages, and the fs is to be reaction 1 hour under 50 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 1.5 hours under 65 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 50% again in reactor, this step reaction divides two stages, and the fs is to be reaction 1.5 hours under 45 ℃ the situation in temperature of reaction, and subordinate phase is to be 1 hour following reaction times of situation of 70 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the oxalic acid solution that adopts 450 mass fractions is neutralization reaction 0.8 hour under 60 ℃ the situation in temperature, is 6 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1.5 hours under the situation of 30 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 4
(1) pulverizes: the refined cellulose process of 1000 mass fractions is pulverized, separated dedusting;
(2) alkalization: the alcoholic solution and the stirring that in reactor, add the 6000-10000 mass fraction, the sheet alkali that adds the 220-250 mass fraction, be warmed up to 70-75 ℃ of choline, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 0.5-1 hour down at 20-30 ℃;
(3) reaction: be divided into for two steps,
The oxyethane that at first in reactor, adds formula ratio 40%-65%, this step reaction divides two stages, fs is to be reaction 0.5-1 hour under 50-55 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 0.5-1 hour under 70-75 ℃ the situation in temperature of reaction;
The oxyethane that in reactor, adds formula ratio 35%-60% then again, this step reaction divides two stages, fs is to be reaction 0.5-1 hour under 50-55 ℃ the situation in temperature of reaction, and subordinate phase is to be 0.5-1 hour following reaction times of situation of 70-75 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the acid solution that adopts the 350-450 mass fraction is under 40-60 ℃ the situation neutralization reaction 0.5-1 hour in temperature, with the pH value of adjusting gained solution between 5.5-8.5;
(5) flash liberation: separate making solid materials enter the washing still, liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1-2 hour under temperature 20-35 ℃ situation in the washing still;
(7) secondary separation: the solid-liquid separation in the washing still, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 5
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: in reactor, add the n-propyl alcohol solution and the stirring of 6000 mass fractions, add the sheet alkali of 220 mass fractions, be warmed up to 70 ℃ of cholines, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 1 hour down at 25 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 45% in reactor, this step reaction divides two stages, and the fs is to be reaction 1 hour under 50 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 1 hour under 70 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 55% again in reactor, this step reaction divides two stages, and the fs is to be reaction 0.5 hour under 55 ℃ the situation in temperature of reaction, and subordinate phase is to be 1 hour following reaction times of situation of 70 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the hydrochloric acid soln that adopts 350 mass fractions is neutralization reaction 0.6 hour under 45 ℃ the situation in temperature, is 8.5 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1.5 hours under the situation of 30 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 6
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: in reactor, add the aqueous isopropanol and the stirring of 10000 mass fractions, add the sheet alkali of 240 mass fractions, be warmed up to 70 ℃ of cholines, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 0.5 hour down at 20 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 40% in reactor, this step reaction divides two stages, and the fs is to be reaction 1 hour under 50 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 1 hour under 70 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 60% again in reactor, this step reaction divides two stages, and the fs is to be reaction 0.5 hour under 55 ℃ the situation in temperature of reaction, and subordinate phase is to be 1 hour following reaction times of situation of 75 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the acetum that adopts 400 mass fractions is neutralization reaction 0.5 hour under 40 ℃ the situation in temperature, is 5.5 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 2 hours under the situation of 20 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 7
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: in reactor, add the n-propyl alcohol solution and the stirring of 8000 mass fractions, add the sheet alkali of 250 mass fractions, be warmed up to 70 ℃ of cholines, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 1 hour down at 30 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 65% in reactor, this step reaction divides two stages, and the fs is to be reaction 1 hour under 55 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 0.5 hour under 75 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 35% again in reactor, this step reaction divides two stages, and the fs is to be reaction 0.5 hour under 55 ℃ the situation in temperature of reaction, and subordinate phase is to be 1 hour following reaction times of situation of 75 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the hydrochloric acid soln that adopts 450 mass fractions is neutralization reaction 1 hour under 50 ℃ the situation in temperature, is 7 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1 hour under the situation of 35 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 8
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: in reactor, add the butanol solution and the stirring of 10000 mass fractions, add the sheet alkali of 250 mass fractions, be warmed up to 70 ℃ of cholines, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 1 hour down at 25 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 50% in reactor, this step reaction divides two stages, and the fs is to be reaction 0.6 hour under 52 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 1 hour under 70 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 50% again in reactor, this step reaction divides two stages, and the fs is to be reaction 0.5 hour under 52 ℃ the situation in temperature of reaction, and subordinate phase is to be 1 hour following reaction times of situation of 72 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the oxalic acid solution that adopts 450 mass fractions is neutralization reaction 0.8 hour under 60 ℃ the situation in temperature, is 6 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1.5 hours under the situation of 30 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 9
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: add the n-propyl alcohol solution and the stirring of 7000 mass fractions in reactor, add the sheet alkali of 200 mass fractions, be warmed up to 70 ℃ of cholines, choline cools to normal temperature after finishing, and adds step
(1) the pulverizing refined cellulose that obtains in alkalized 1 hour down at 25 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 45% in reactor, this step reaction divides two stages, and the fs is to be reaction 1 hour under 50 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 1 hour under 70 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 55% again in reactor, this step reaction divides two stages, and the fs is to be reaction 0.5 hour under 55 ℃ the situation in temperature of reaction, and subordinate phase is to be 1 hour following reaction times of situation of 70 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the hydrochloric acid soln that adopts 400 mass fractions is neutralization reaction 0.6 hour under 45 ℃ the situation in temperature, is 8.5 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1.5 hours under the situation of 30 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Embodiment 10
(1) pulverize: the refined cellulose of 1000 mass fractions is pulverized with rotating knife formula pulverizer, separated through cyclonic separator, reach 0.03-0.15mm (about 80 orders), tail gas is through bag-type dusting;
(2) alkalization: in reactor, add the isobutanol solution and the stirring of 12000 mass fractions, add the sheet alkali of 280 mass fractions, be warmed up to 70 ℃ of cholines, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 1 hour down at 20 ℃;
(3) reaction: be divided into for two steps,
At first, add the oxyethane of formula ratio 60% in reactor, this step reaction divides two stages, and the fs is to be reaction 1 hour under 50 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 0.6 hour under 75 ℃ the situation in temperature of reaction;
Then, add the oxyethane of formula ratio 40% again in reactor, this step reaction divides two stages, and the fs is to be reaction 0.5 hour under 50 ℃ the situation in temperature of reaction, and subordinate phase is to be 1 hour following reaction times of situation of 75 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the phosphoric acid solution that adopts 500 mass fractions is neutralization reaction 1 hour under 60 ℃ the situation in temperature, is 5.5 with the pH value of adjusting gained solution;
(5) flash liberation: use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 2 hours under the situation of 20 ℃ of temperature in the washing still;
(7) secondary separation: use the spiral pump convey materials in the washing still, separate with the horizontal spiral separating machine, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Through experiment repeatedly, all obtain effect preferably, the leading indicator that product reaches is:
Substitution value: 2.0-2.6 improves 10-30% than present common process, reaches external equal quality level.
Transmittance: 85-90% improves 5-15% than present common process, reaches international best level.
Viscosity: NDJ-1 viscosity (2% aqueous solution) 10-50000mPa.s.
Claims (2)
1. a technology of producing the high substitution value Natvosol is characterized in that, realizes by following steps:
(1) pulverizes: the refined cellulose process of 1000 mass fractions is pulverized, separated dedusting;
(2) alkalization: the alcoholic solution and the stirring that in reactor, add the 5000-12000 mass fraction, the sheet alkali that adds the 200-280 mass fraction, be warmed up to 60-85 ℃ of choline, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 0.5-1.5 hour down at 15-35 ℃;
(3) reaction: be divided into for two steps,
The oxyethane that at first in reactor, adds formula ratio 40%-65%, this step reaction divides two stages, fs is to be reaction 0.5-1.5 hour under 45-60 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 0.5-1.5 hour under 65-85 ℃ the situation in temperature of reaction;
The oxyethane that in reactor, adds formula ratio 35%-60% then again, this step reaction divides two stages, fs is to be reaction 0.5-1.5 hour under 45-60 ℃ the situation in temperature of reaction, and subordinate phase is to be 0.5-2 hour following reaction times of situation of 65-85 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the acid solution that adopts the 300-500 mass fraction is under 40-60 ℃ the situation neutralization reaction 0.5-1 hour in temperature, with the pH value of adjusting gained solution between 5.5-8.5;
(5) flash liberation: separate making solid materials enter the washing still, liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1-2 hour under temperature 20-35 ℃ situation in the washing still;
(7) secondary separation: the solid-liquid separation in the washing still, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
2. a kind of technology of producing the high substitution value Natvosol according to claim 1 is characterized in that, realizes by following steps:
(1) pulverizes: the refined cellulose process of 1000 mass fractions is pulverized, separated dedusting;
(2) alkalization: the alcoholic solution and the stirring that in reactor, add the 6000-10000 mass fraction, the sheet alkali that adds the 220-250 mass fraction, be warmed up to 70-75 ℃ of choline, after choline finishes, cool to normal temperature, add the pulverizing refined cellulose that obtains in the step (1), alkalized 0.5-1 hour down at 20-30 ℃;
(3) reaction: be divided into for two steps,
The oxyethane that at first in reactor, adds formula ratio 40%-65%, this step reaction divides two stages, fs is to be reaction 0.5-1 hour under 50-55 ℃ the situation in temperature of reaction, and subordinate phase is to be reaction 0.5-1 hour under 70-75 ℃ the situation in temperature of reaction;
The oxyethane that in reactor, adds formula ratio 35%-60% then again, this step reaction divides two stages, fs is to be reaction 0.5-1 hour under 50-55 ℃ the situation in temperature of reaction, and subordinate phase is to be 0.5-1 hour following reaction times of situation of 70-75 ℃ in temperature of reaction;
Above-mentioned two-step reaction process is controlled by computer program;
(4) neutralization: the acid solution that adopts the 350-450 mass fraction is under 40-60 ℃ the situation neutralization reaction 0.5-1 hour in temperature, with the pH value of adjusting gained solution between 5.5-8.5;
(5) flash liberation: separate making solid materials enter the washing still, liquid solvent recycles through the evaporation of solvent evaporation device;
(6) washing: solid materials washed 1-2 hour under temperature 20-35 ℃ situation in the washing still;
(7) secondary separation: the solid-liquid separation in the washing still, solid materials enters the washing still, and liquid solvent recycles through the evaporation of solvent evaporation device;
(8) drying: crushed after being dried packing.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110077321 CN102180978A (en) | 2011-03-23 | 2011-03-23 | Technology for producing substitution-degree hydroxyethyl cellulose |
| CN2012100345135A CN102532327A (en) | 2011-03-23 | 2012-02-16 | Process for producing hydroxyethyl cellulose with high degree of substitution |
Applications Claiming Priority (1)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532327A (en) * | 2011-03-23 | 2012-07-04 | 刘传荣 | Process for producing hydroxyethyl cellulose with high degree of substitution |
| CN102603899A (en) * | 2012-02-24 | 2012-07-25 | 邸勇 | Process for producing low-substituted hydroxypropyl cellulose |
| CN102617741A (en) * | 2012-02-24 | 2012-08-01 | 刘传荣 | Process for producing hydroxy propyl cellulose with high substitution degree |
| CN102643356A (en) * | 2012-03-20 | 2012-08-22 | 邸勇 | Two-step production process of ethyl cellulose with high degree of substitution |
| CN102807624A (en) * | 2012-05-21 | 2012-12-05 | 新疆光大山河化工科技有限公司 | Preparation technology of hydroxypropyl methylcellulose ether (HPMC) |
| CN102911272A (en) * | 2012-11-15 | 2013-02-06 | 泰安赛露纤维素醚科技有限公司 | Process for producing hydroxyethyl cellulose with high degree of substitution by binary complex solvent |
| CN106632698A (en) * | 2016-12-19 | 2017-05-10 | 扬州中福生物技术有限公司 | Preparation method for producing high-substitution-degree HEC (Hydroxy Ethyl Cellulose) by adopting TBA (Tert-butyl Alcohol) process |
| CN104837869B (en) * | 2012-12-06 | 2017-10-27 | 花王株式会社 | Method for preparing hydroxy alkyl cellulose |
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| CN101250230A (en) * | 2008-03-10 | 2008-08-27 | 江苏飞翔化工股份有限公司 | Method for preparing hydroxyethyl cellulose |
| CN101864607A (en) * | 2010-06-23 | 2010-10-20 | 东华大学 | Method for preparing hydroxyethyl cellulose |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102180978A (en) * | 2011-03-23 | 2011-09-14 | 刘传荣 | Technology for producing substitution-degree hydroxyethyl cellulose |
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| CN1174202A (en) * | 1996-08-15 | 1998-02-25 | 鞠馥阳 | Ethoxyl cellulose producing process from plant cotton |
| CN1673233A (en) * | 2004-03-23 | 2005-09-28 | 刘延金 | Carboxymethyl hydroxyethyl cellulose producing process |
| CN101250230A (en) * | 2008-03-10 | 2008-08-27 | 江苏飞翔化工股份有限公司 | Method for preparing hydroxyethyl cellulose |
| CN101864607A (en) * | 2010-06-23 | 2010-10-20 | 东华大学 | Method for preparing hydroxyethyl cellulose |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532327A (en) * | 2011-03-23 | 2012-07-04 | 刘传荣 | Process for producing hydroxyethyl cellulose with high degree of substitution |
| CN102603899A (en) * | 2012-02-24 | 2012-07-25 | 邸勇 | Process for producing low-substituted hydroxypropyl cellulose |
| CN102617741A (en) * | 2012-02-24 | 2012-08-01 | 刘传荣 | Process for producing hydroxy propyl cellulose with high substitution degree |
| CN102643356A (en) * | 2012-03-20 | 2012-08-22 | 邸勇 | Two-step production process of ethyl cellulose with high degree of substitution |
| CN102807624A (en) * | 2012-05-21 | 2012-12-05 | 新疆光大山河化工科技有限公司 | Preparation technology of hydroxypropyl methylcellulose ether (HPMC) |
| CN102807624B (en) * | 2012-05-21 | 2015-02-11 | 新疆光大山河化工科技有限公司 | Preparation technology of hydroxypropyl methylcellulose ether (HPMC) |
| CN102911272A (en) * | 2012-11-15 | 2013-02-06 | 泰安赛露纤维素醚科技有限公司 | Process for producing hydroxyethyl cellulose with high degree of substitution by binary complex solvent |
| CN104837869B (en) * | 2012-12-06 | 2017-10-27 | 花王株式会社 | Method for preparing hydroxy alkyl cellulose |
| CN106632698A (en) * | 2016-12-19 | 2017-05-10 | 扬州中福生物技术有限公司 | Preparation method for producing high-substitution-degree HEC (Hydroxy Ethyl Cellulose) by adopting TBA (Tert-butyl Alcohol) process |
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| CN102532327A (en) | 2012-07-04 |
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