CN102718874B - Method for preparing methyl cellulose ether with arundodomax dissolving pulp serving as raw material - Google Patents
Method for preparing methyl cellulose ether with arundodomax dissolving pulp serving as raw material Download PDFInfo
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Abstract
The invention discloses a method for preparing methyl cellulose ether with arundodomax dissolving pulp serving as a raw material. The method comprises the following steps of: adding arundodomax dissolving pulp powder into a mixture of ethanol and sodium hydroxide, and alkalizing the powder and the mixture to obtain sodium carboxymethyl cellulose; adding etherifying agent in the sodium carboxymethyl cellulose for etherifying with a combined catalyst, and then collecting reacting liquid, and soaking the reacting liquid through acid solution, and centrifugally separating the reacting liquid to remove acid solution; washing the liquid through water, and removing moisture in the liquid; and drying the liquid, and then crashing and refining the liquid to obtain the methyl cellulose ether. According to the method disclosed by the invention, the existing and conventional technology for producing the methyl cellulose is changed, a combined catalyzing method with solid base is introduced for etherifying, therefore, the temperature in etherification is lowered, the etherification time is reduced, the corrosion on production equipment is reduced, the energy consumption is reduced, and waste liquid produced in the production process is obviously decreased. The method requires small investment, is simple in technology, is particularly suitable for serving as a processing technology in a producing area of the arundodomax, and provides new raw materials for building motor and papermaking.
Description
Technical field
The present invention relates to the preparation method of methyl cellulose ether, be specifically related to take giantreed dissolving pulp and prepare the method for methyl cellulose ether as raw material.
Background technology
Giantreed is widely distributed in China, North gets Liaoning, reaches Guangxi in the south, and producing maximum is riverine sea wall band, and to administering environment and the anti-landslide face of flood control, giantreed has been brought into play unique effect.Giantreed growth is simultaneously fast, and adaptive faculty is very strong, is also easy to breeding, has good economic worth.Yet owing to being subject to impact and the restriction of the many factors such as environment protection and Economic development imbalance, China is also in the low-level stage in the comprehensive utilization of giantreed, and a large amount of giantreeds can only be used as fuel, does not bring into play due economic worth.Therefore utilize environment and the geography of giantreed growth, improve the economic worth of giantreed comprehensive utilization, give full play to gather materials on the spot, reduce costs, a major issue that protection of the environment is giantreed processing technology.
High speed development along with Chinese national economy, the demand of ether of cellulose constantly rises, be mainly used in the industries such as building, papermaking, food, medicine, petrochemical industry, the cotton price of using due to production of cellulose ether rises steadily, cause the continuous increase of ether of cellulose production cost, increased the weight of the burden of enterprise.
Current production of cellulose ether main raw material or cotton is main, though there are wood pulp for patent Introduction or bamboo pulp to replace the method for Cotton Production ether of cellulose, because of severe reaction conditions and the high object that does not reach expection of equipment manufacturing cost.
Summary of the invention
The object of this invention is to provide and a kind ofly take giantreed dissolving pulp and prepare the method for methyl cellulose ether as raw material, for overcoming the defect of prior art.
Method of the present invention, comprises the steps:
(a). giantreed is dissolved to starch, and to add volumetric concentration be 75～95% ethanol and the mixture of sodium hydroxide, and 20 ℃-40 ℃ alkalization 2-3 hour, obtain sodium cellulosate;
The granularity that described giantreed is dissolved starch is 200-300 μ m;
The parts by weight of component are:
Volumetric concentration is 100 parts of 75～95% ethanol
Giantreed is dissolved 20～30 parts of starches
10～15 parts, sodium hydroxide
(b). described sodium cellulosate is added to etherifying agent, under combination catalyst exists, etherification reaction 1-2 hour at 45 ℃ of-60 ℃ of temperature, then separating reaction liquid and reclaim catalyzer, with the acid solution of 85 ℃-95 ℃, soak 30-60 minute, then acid solution is removed in centrifugation;
Described acid solution is the acetum of weight concentration 1% or the sulphuric acid soln of weight concentration 0.5%;
Described etherifying agent is one or several in monochloro methane, methylene dichloride or trichloromethane;
Described combination catalyst comprises the component of following weight percent:
Solid super base 98～99%
Nanometer cuprous chloride 0.5～1%
Nano silver/silver chloride 0.5～1%
Preferably:
Solid super base 99%
Nanometer cuprous chloride 0.5%
Nano silver/silver chloride 0.5%
The particle diameter of nanometer cuprous chloride, nano silver/silver chloride is 20～40 nanometers; Select excellent 30 nanometers, described solid super strong alkali preparation method is as follows:
By 4 grams of nitrate of baryta, 4.3 grams of Magnesium dichloride hexahydrates and 0.5 gram of rubidium nitrate join in 400 milliliters of dehydrated alcohols and 50 milliliters of dioxane mixed solvents, ultrasonic dispersion 30 minutes, stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 grams of polyvinyl alcohol 800 aqueous solution, continue to stir 4 hours, the whole solvents of slow evaporation at 90 ℃, at 500 ℃, roasting is 2 hours, obtain solid super base, adopt the method for Chinese patent CN200510011269.0 report.
(c.) water washing with 85 ℃-95 ℃ by the product of step b, the centrifugal moisture content of removing;
(d.) by the product of step c, 90～110 ℃ are dry, and to control water content be 1-2%, dispersion and fining then, and granularity is 60-80 μ m, obtains described methyl cellulose ether;
The production method of described giantreed dissolving pulp, comprises the steps;
(1) giantreed is crushed, pulverize segment, length is 3 ~ 5cm;
(2) by the washing of giantreed tablet, remove plaster dirt, dress pot;
(3) giantreed sheet is added to hydrating solution, in solid acid catalyst, soak 30-60 minute, hydrating solution weight is 1.5～2: 1 with the ratio of giantreed tablet weight;
The weight consumption of solid acid catalyst is 5～15% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2type solid acid catalyst, is comprised of the element sulphur of more than 90% zirconium dioxide and 0.1～0.5% platinum and 0.5～5%, and median size is 20 nanometers, and by being processed into agglomeration sphere-like, sphere diameter is 4～6mm conventionally.
Preparation by the following method:
By ZrOCl
2ammoniacal liquor with 25% is hydrolyzed 2 hours (PH is controlled at 10) at 50 ℃, generates after zirconium hydroxide, use again 90 ℃ of deionized water soaking and washing 10 hours, then filter, then clean with 90 ℃ of deionized waters, after refiltering, at 110 ℃, be dried 10 hours, at 680 ℃, roasting is 5 hours, then soaks 3 hours with being mixed with in 1% dilute sulphuric acid and 1.67% ammonium chloroplatinate mixed solution, at 110 ℃ dry 3 hours, roasting 4 hours at 680 ℃ again, makes solid super-strong acid.(referring to Teaching Materials at College level < < chemical functional materials outline > > mono-book)
Solid acid catalyst is selected from the SO of the positive big vast biofuel equipment of Wuxi City Science and Technology Ltd.
4 2--ZrO
2type solid acid catalyst.
(4) then by whole materials of step (3), at the temperature of 130 ℃-150 ℃, boiling 30-60 minute;
(5) be warming up to 160 ℃-180 ℃, continue to keep 30-60 minute;
(6) venting, reclaims respectively boiling slurry and solid acid catalyst, and boiling slurry cleans with the water of 80-90 ℃;
(7) in boiling slurry, adding weight concentration is 5-10% sodium hydroxide solution, soaks 30-60 minute, and then boiling 30-60 minute at 130 ℃-150 ℃, reclaims boiling slurry 2 times;
The weight consumption of described sodium hydroxide solution, in sodium hydroxide, is 5～6% of raw material giantreed tablet;
(8) Sulfothiorine and superoxol are added to boiling slurry 2 times, then add water to slurry and flood, pass into steam, be warming up to 90 ℃-120 ℃, bleaching 30-60 minute, reclaims bleaching slurry; Giantreed dissolving pulp for preliminary working;
The weight consumption of component is:
Raw material giantreed tablet: Sulfothiorine=1:0.05～0.15;
Raw material giantreed tablet: 30% hydrogen peroxide=1:0.2～0.4
Described giantreed dissolving pulp, for the preparation of ether of cellulose or paper making raw material.
The invention has the advantages that and utilized resourceful giantreed for raw material; by giantreed production preliminary working, become dissolving pulp; ether of cellulose is produced in regeneration; changed the traditional technology that existing ether of cellulose is produced; introduce solid alkali assembly catalyze method and carry out etherification reaction; not only reduce the temperature of etherification reaction but also shortened time of etherification reaction; reduced in process of production the corrosion to production unit; reduced energy consumption; significantly reduce the waste liquid producing in production process; improved the effective utilization to water resources, protection of the environment particular significant effect.The present invention invests little, and technique is simple, is particularly suitable for giantreed place of production processing technology, for building mortar, papermaking have increased new raw material.
Embodiment
Embodiment 1
One, giantreed dissolving pulp is produced the method for methyl cellulose ether:
(a). in 100 parts of 95% ethanol, 10 parts, sodium hydroxide, heats and makes dissolution of sodium hydroxide, adds giantreed to dissolve 20 parts of starches, at 20 ℃, stirs alkalization 3 hours, makes it to generate sodium cellulosate.
The granularity that giantreed is dissolved starch is 200 μ m;
The parts by weight of component are:
Volumetric concentration is 100 parts of 95% ethanol
Giantreed is dissolved 20 parts of starches
10 parts, sodium hydroxide
(b). will in described sodium cellulosate, add etherifying agent, under the existence of combination catalyst, at 45 ℃ of temperature, etherification reaction is 2 hours, then separating reaction liquid and reclaim combination catalyst, 100 parts of immersions of the acetum that is 1% by the weight concentrations of 95 ℃ 30 minutes, then remove acid solution with whizzer;
Described etherifying agent is monochloro methane;
The components by weight percent of catalyzer: 99% solid super base, 0.5% nanometer cuprous chloride, 0.5% nano silver/silver chloride; Catalyzer is coated with 300 object stainless (steel) wires.
The preparation method of solid super base: by 4 grams of nitrate of baryta, 4.3 grams of Magnesium dichloride hexahydrates and 0.5 gram of rubidium nitrate join in 400 milliliters of dehydrated alcohols and 50 milliliters of dioxane mixed solvents, ultrasonic dispersion 30 minutes, stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 grams of polyvinyl alcohol 800 aqueous solution, continue to stir 4 hours, the whole solvents of slow evaporation at 90 ℃, at 500 ℃, roasting is 2 hours, obtain solid super base, adopt the method for Chinese patent CN200510011269.0 report.
The particle diameter of nanometer cuprous chloride, nano silver/silver chloride is 20～40 nanometers; Preferred 30 nanometers.
(c.) with 95 ℃ of deionized waters, clean the remaining acid solution in ether of cellulose surface, then with the centrifugal moisture content of removing of whizzer;
(d) product of step c is dried at 90 ℃, controlling water content is 1%, then with pulverizer by ether of cellulose refinement, controlling average particle size is 60 μ m, obtains described methyl cellulose ether.
Two, the production method of giantreed dissolving pulp:
(a) giantreed is crushed, pulverize segment, mean length is 3cm;
(b) by the washing of giantreed tablet, remove plaster dirt, dress pot;
(c) giantreed sheet is added to hydrating solution, in solid acid catalyst, soak 30 minutes, hydrating solution weight is 1.5: 1 with the ratio of giantreed tablet weight;
The weight consumption of solid acid catalyst is 5% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2type solid acid catalyst, is comprised of the element sulphur of more than 90% zirconium dioxide and 0.1～0.5% platinum and 0.5～5%, and median size is 20 nanometers, and by being processed into agglomeration sphere-like, sphere diameter is 4～6mm conventionally.
Preparation by the following method:
By ZrOCl
2ammoniacal liquor with 25% is hydrolyzed 2 hours (PH is controlled at 10) at 50 ℃, generates after zirconium hydroxide, use again 90 ℃ of deionized water soaking and washing 10 hours, then filter, then clean with 90 ℃ of deionized waters, after refiltering, at 110 ℃, be dried 10 hours, at 680 ℃, roasting is 5 hours, then soaks 3 hours with being mixed with in 1% dilute sulphuric acid and 1.67% ammonium chloroplatinate mixed solution, at 110 ℃ dry 3 hours, roasting 4 hours at 680 ℃ again, makes solid super-strong acid.
(d) then by whole materials of step (3), at 130 ℃, boiling 30 minutes;
(e) be warming up at 160 ℃ and continue to keep 30 minutes;
(f) venting, reclaims respectively boiling slurry and solid acid catalyst, and boiling slurry cleans with the water of 80 ℃;
(g) in boiling slurry, adding weight concentration is 5% sodium hydroxide solution, soaks 30 minutes, and then, at 130 ℃, boiling 30 minutes, reclaims boiling slurry 2 times;
The weight consumption of sodium hydroxide solution, in sodium hydroxide, is 5% of raw material giantreed tablet;
(h) Sulfothiorine and superoxol are added to boiling slurry 2 times, then add water to slurry and flood, pass into steam, be warming up to 90 ℃, bleach 30 minutes, reclaim bleaching slurry; For the giantreed dissolving pulp of preliminary working, for the preparation of ether of cellulose.
The weight consumption of component is:
Raw material giantreed tablet: Sulfothiorine=1:0.05, raw material giantreed tablet: 30% hydrogen peroxide=1:0.2
Embodiment 2
One, giantreed dissolving pulp is produced the method for methyl cellulose ether:
(a). in 100 parts of 85% ethanol, 15 parts, sodium hydroxide, heats and makes dissolution of sodium hydroxide, adds giantreed to dissolve 30 parts of starches, at 40 ℃, stirs alkalization 2 hours, makes it to generate sodium cellulosate.
The granularity that giantreed is dissolved starch is 300 μ m;
The parts by weight of component are:
Volumetric concentration is 100 parts of 85% ethanol
30 parts of giantreed dissolving pulps
15 parts, sodium hydroxide
(b). described sodium cellulosate is added to etherifying agent, under the catalyzer of combination exists, at 45 ℃ of ℃ of temperature, etherification reaction is 1 hour, then separating reaction liquid and recovery combination catalyst, by the weight concentrations of 95 ℃, be that 100 parts of 0.5% sulphuric acid solns soak 60 minutes, then remove acid solution with whizzer;
Described etherifying agent be methylene dichloride,
Combination catalyst component: 99% solid super base, 0.5% nanometer cuprous chloride, 0.5% nano silver/silver chloride; Catalyzer is coated with 300 object stainless (steel) wires.
The preparation method of solid super base: by 4 grams of nitrate of baryta, 4.3 grams of Magnesium dichloride hexahydrates and 0.5 gram of rubidium nitrate join in 400 milliliters of dehydrated alcohols and 50 milliliters of dioxane mixed solvents, ultrasonic dispersion 30 minutes, stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 grams of polyvinyl alcohol 800 aqueous solution, continue to stir 4 hours, the whole solvents of slow evaporation at 90 ℃, at 500 ℃, roasting is 2 hours, obtain solid super base, adopt the method for Chinese patent CN200510011269.0 report.
The particle diameter of nanometer cuprous chloride, nano silver/silver chloride is 20 nanometers.
(c). with 85 ℃ of deionized waters, clean the remaining acid solution in ether of cellulose surface, then with the centrifugal moisture content of removing of whizzer, (d) product of step c is dried at 100 ℃, controlling water content is 2%, again with pulverizer by ether of cellulose refinement, controlling average particle size is 80 μ m, is product.
Two, the production method of giantreed dissolving pulp:
(a) giantreed is crushed, pulverize segment, mean length is 5cm;
(b) by the washing of giantreed tablet, remove plaster dirt, dress pot;
(c) giantreed sheet is added to hydrating solution, in solid acid catalyst, soak 60 minutes, hydrating solution weight is 2: 1 with the ratio of giantreed tablet weight;
The weight consumption of solid acid catalyst is 15% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2type solid acid catalyst, is comprised of the element sulphur of more than 90% zirconium dioxide and 0.1～0.5% platinum and 0.5～5%, and median size is 20 nanometers, and by being processed into agglomeration sphere-like, sphere diameter is 4～6mm conventionally.
Preparation by the following method:
By ZrOCl
2ammoniacal liquor with 25% is hydrolyzed 2 hours (PH is controlled at 10) at 50 ℃, generates after zirconium hydroxide, use again 90 ℃ of deionized water soaking and washing 10 hours, then filter, then clean with 90 ℃ of deionized waters, after refiltering, 110 ℃ dry 10 hours, at 680 ℃, roasting is 5 hours, then soaks 3 hours with being mixed with in 1% dilute sulphuric acid and 1.67% ammonium chloroplatinate mixed solution, after refiltering, at 110 ℃ dry 3 hours, then roasting 4 hours at 680 ℃, solid super-strong acid made.
(d) then by whole materials of step (3), at 150 ℃, boiling 60 minutes;
(e) be warming up to 180 ℃, continue to keep 60 minutes;
(f) venting, reclaims respectively boiling slurry and solid acid catalyst, and boiling slurry cleans with the water of 80-90 ℃;
(g) in boiling slurry, adding weight concentration is 10% sodium hydroxide solution, soaks 60 minutes, and then 150 ℃, boiling 30 minutes, reclaims boiling slurry 2 times;
The weight consumption of sodium hydroxide solution, in sodium hydroxide, is 6% of raw material giantreed tablet;
(h) Sulfothiorine and superoxol are added to boiling slurry 2 times, then add water to slurry and flood, pass into steam, be warming up to 120 ℃, bleach 60 minutes, reclaim bleaching slurry; Giantreed dissolving pulp for preliminary working;
The weight consumption of component is:
Raw material giantreed tablet: Sulfothiorine=1:0.1; Raw material giantreed tablet: 30% hydrogen peroxide=1:0.4.
Embodiment 3
One, giantreed dissolving pulp is produced the method for methyl cellulose ether, by following steps:
(a). in 100 parts of 75% ethanol, 12.5 parts, sodium hydroxide, heats and makes dissolution of sodium hydroxide, adds giantreed to dissolve 25 parts of starches, at 30 ℃, stirs alkalization 2.5 hours, makes it to generate sodium cellulosate.
The granularity that giantreed is dissolved starch is 250 μ m;
The parts by weight of component are:
Volumetric concentration is 100 parts of 75% ethanol
Giantreed is dissolved 25 parts of starches
12.5 parts, sodium hydroxide
(b). described sodium cellulosate is added to etherifying agent, under the catalyzer of combination exists, at 45 ℃ of temperature, etherification reaction is 2 hours, then separating reaction liquid and recovery combination catalyst, by the weight concentrations of 95 ℃, be that 100 parts of 1% acetums soak 45 minutes, then remove acid solution with whizzer;
Described etherifying agent is trichloromethane;
Combination catalyst component: 99% solid super base, 0.5% nanometer cuprous chloride, 0.5% nano silver/silver chloride; Catalyzer is coated with 300 object stainless (steel) wires.
The preparation method of solid super base: by 4 grams of nitrate of baryta, 4.3 grams of Magnesium dichloride hexahydrates and 0.5 gram of rubidium nitrate join in 400 milliliters of dehydrated alcohols and 50 milliliters of dioxane mixed solvents, ultrasonic dispersion 30 minutes, stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 grams of polyvinyl alcohol 800 aqueous solution, continue to stir 4 hours, the whole solvents of slow evaporation at 90 ℃, at 500 ℃, roasting is 2 hours, obtain solid super base, adopt the method for Chinese patent CN200510011269.0 report.
The particle diameter of nanometer cuprous chloride, nano silver/silver chloride is 20 nanometers.
﹙ c ﹚ cleans the remaining acid solution in ether of cellulose surface with 90 ℃ of deionized waters, then with the centrifugal moisture content of removing of whizzer,
﹙ d ﹚ is dried the product of the poly-c of step at 110 ℃, and controls water content is 1-2%, then with pulverizer by ether of cellulose refinement, control average particle size is 80 μ m, is product.
Two, the production method of giantreed dissolving pulp
(a) giantreed is crushed, pulverize segment, mean length is 4cm;
(b) by the washing of giantreed tablet, remove plaster dirt, dress pot;
(c) giantreed sheet is added to hydrating solution, in solid acid catalyst, soak hydrating solution weight and giantreed 50 minutes
The ratio of tablet weight is 1.75: 1;
The weight consumption of solid acid catalyst is 10% of giantreed tablet;
The parts by weight of described hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2type solid acid catalyst, is comprised of the element sulphur of more than 90% zirconium dioxide and 0.1～0.5% platinum and 0.5～5%, and median size is 20 nanometers, and by being processed into agglomeration sphere-like, sphere diameter is 4～6mm conventionally.
Preparation by the following method:
By ZrOCl
2ammoniacal liquor with 25% is hydrolyzed 2 hours (PH is controlled at 10) at 50 ℃, generates after zirconium hydroxide, use again 90 ℃ of deionized water soaking and washing 10 hours, then filter, then clean with 90 ℃ of deionized waters, after refiltering, at 110 ℃, be dried 10 hours, at 680 ℃, roasting is 5 hours, then soaks 3 hours with being mixed with in 1% dilute sulphuric acid and 1.67% ammonium chloroplatinate mixed solution, at 110 ℃ dry 3 hours, roasting 4 hours at 680 ℃ again, makes solid super-strong acid.
(d) then by whole materials of step (3) (comprising giantreed tablet, hydrating solution and solid acid catalyst), at 140 ℃, boiling 45 minutes;
(e) be warming up at 170 ℃ and continue to keep 50 minutes;
(f) venting, reclaims respectively boiling slurry and solid acid catalyst, and boiling slurry cleans with the water of 80-90 ℃;
(g) in boiling slurry, adding weight concentration is 8% sodium hydroxide solution, soaks 45 minutes, and then 140 ℃, boiling 45 minutes, reclaims boiling slurry 2 times;
The weight consumption of sodium hydroxide solution, in sodium hydroxide, is 5.5% of raw material giantreed tablet;
(h) Sulfothiorine and superoxol are added to boiling slurry 2 times, then add water to slurry and flood, pass into steam, be warming up to 105 ℃, bleach 45 minutes, reclaim bleaching slurry; Giantreed dissolving pulp for preliminary working;
The weight consumption of component is:
Raw material giantreed tablet: Sulfothiorine=1:0.15, raw material giantreed tablet: 30% hydrogen peroxide=1:0.3.
Embodiment 4
One, giantreed dissolving pulp is produced the method for methyl cellulose ether:
(a). in 100 parts of 90% ethanol, 15 parts, sodium hydroxide, heats and makes dissolution of sodium hydroxide, adds giantreed to dissolve 30 parts of starches, at 40 ℃, stirs alkalization 2 hours, makes it to generate sodium cellulosate.
The granularity that giantreed is dissolved starch is 300 μ m;
The parts by weight of component are:
Volumetric concentration is 100 parts of 85% ethanol
Giantreed is dissolved 30 parts of starches
15 parts, sodium hydroxide
(b). described sodium cellulosate is added to etherifying agent, under the catalyzer of combination exists, at 45 ℃ of temperature, etherification reaction is 1 hour, then separating reaction liquid and recovery combination catalyst, 100 parts of immersions of the sulphuric acid soln that is 0.5% by 95 ℃ of weight concentrations 60 minutes, then remove acid solution with whizzer;
Described etherifying agent is respectively 5 parts of a monochloro methane, methylene dichloride, trichloromethanes;
Combination catalyst component: 99% solid super base, 0.5% nanometer cuprous chloride, 0.5% nano silver/silver chloride; Catalyzer is coated with 300 object stainless (steel) wires.
The preparation method of solid super base: by 4 grams of nitrate of baryta, 4.3 grams of Magnesium dichloride hexahydrates and 0.5 gram of rubidium nitrate join in 400 milliliters of dehydrated alcohols and 50 milliliters of dioxane mixed solvents, ultrasonic dispersion 30 minutes, stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 grams of polyvinyl alcohol 800 aqueous solution, continue to stir 4 hours, the whole solvents of slow evaporation at 90 ℃, at 500 ℃, roasting is 2 hours, obtain solid super base, adopt the method for Chinese patent CN200510011269.0 report.
The particle diameter of nanometer cuprous chloride, nano silver/silver chloride is 40 nanometers;
﹙ c ﹚ cleans the remaining acid solution in ether of cellulose surface with 95 ℃ of deionized waters, then with the centrifugal moisture content of removing of whizzer,
The product that ﹙ d ﹚ rises step c is dried at 100 ℃, and control water content is 1-2%, then with pulverizer by ether of cellulose refinement, control average particle size at 70 μ m.
Two, the production method of giantreed dissolving pulp is with embodiment 1.
Being determined as follows of embodiment ether of cellulose:
The effect of embodiment ether of cellulose in sand-cement slurry: reference standard JC/T992-2006
From the effect sand-cement slurry, judge that methyl cellulose ether of the present invention reaches the effect with the ether of cellulose of Cotton Production completely.
Claims (1)
1. the giantreed dissolving pulp of take is prepared the method for methyl cellulose ether as raw material, it is characterized in that, comprises the steps:
(a). giantreed is dissolved to the mixture that starch adds ethanol and sodium hydroxide, and alkalization, obtains sodium cellulosate;
(b). described sodium cellulosate is added to etherifying agent, and under combination catalyst exists, etherification reaction, then collects reaction solution, with acid solution, soaks, and acid solution is removed in centrifugation;
(c.) product of step b is washed with water, remove moisture content;
(d.), by the product of step c, dry, then dispersion and fining, obtains described methyl cellulose ether;
In step (a), the parts by weight of component are:
Volumetric concentration is 100 parts of 75～95% ethanol
Giantreed is dissolved 20～30 parts of starches
10～15 parts, sodium hydroxide;
In step (b), described sodium cellulosate is added to etherifying agent, under combination catalyst exists, etherification reaction 1-2 hour at 45 ℃ of-60 ℃ of temperature, then collect reaction solution, with the acid solutions of 85 ℃-95 ℃, soak 30-60 minute, acid solution is removed in centrifugation;
The parts by weight of each component are:
Described acid solution is the acetum of weight concentration 1% or the sulphuric acid soln that weight concentration is 0.5%;
Described etherifying agent is one or several in monochloro methane, methylene dichloride or trichloromethane;
Described combination catalyst comprises the component of following weight percent:
Solid super base 98～99%
Nanometer cuprous chloride 0.5～1%
Nano silver/silver chloride 0.5～1%;
Described solid super strong alkali preparation method is as follows:
By 4 grams of nitrate of baryta, 4.3 grams of Magnesium dichloride hexahydrates and 0.5 gram of rubidium nitrate join in 400 milliliters of dehydrated alcohols and 50 milliliters of dioxane mixed solvents, ultrasonic dispersion 30 minutes, stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 grams of polyvinyl alcohol 800 aqueous solution, continue to stir 4 hours, the whole solvents of slow evaporation at 90 ℃, at 500 ℃, roasting is 2 hours, obtains solid super base.
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| CN103232546A (en) * | 2013-04-28 | 2013-08-07 | 河北金源同舟化工科技有限公司 | Cellulose ether and method for producing same from bamboo pulp |
| CN103483456B (en) * | 2013-10-15 | 2016-03-30 | 湖北博斐逊生物新材料有限公司 | A kind of preparation method of cement fiber sizing and the application in cement products thereof |
| CN105017431A (en) * | 2015-08-19 | 2015-11-04 | 昆山京昆油田化学科技开发公司 | Synthetic method for methyl cellulose sample |
| EP3692076A1 (en) * | 2017-10-03 | 2020-08-12 | Dow Global Technologies LLC | Simplified process for making low viscosity cellulose ether |
| CN111320705A (en) * | 2020-04-26 | 2020-06-23 | 山东洲星天然物提取智能设备有限公司 | Preparation method of high-viscosity cellulose ether |
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|---|---|---|---|---|
| CN102101891A (en) * | 2011-03-31 | 2011-06-22 | 河北吉藁化纤有限责任公司 | Cellulose ether and preparation method thereof |
| CN102127170A (en) * | 2011-03-23 | 2011-07-20 | 山东一滕化工有限公司 | Method for preparing cellulose ether by utilizing wood pulp |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102127170A (en) * | 2011-03-23 | 2011-07-20 | 山东一滕化工有限公司 | Method for preparing cellulose ether by utilizing wood pulp |
| CN102101891A (en) * | 2011-03-31 | 2011-06-22 | 河北吉藁化纤有限责任公司 | Cellulose ether and preparation method thereof |
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