CN102718874A - 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, being specifically related to the giantreed dissolving pulp is the method for feedstock production methyl cellulose ether.
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 simultaneously is fast, and adaptive faculty is very strong, also is easy to breeding, has good economic worth.Yet owing to receive influence of various factors and restrictions such as environment protection and Economic development imbalance, China also is in the low-level stage in the comprehensive utilization of giantreed, and due economic worth is not brought into play in the use that can only act as a fuel of a large amount of giantreeds.Therefore utilize the environment and the geography of giantreed growth, improve the economic worth of giantreed comprehensive utilization, giving full play to and gathering materials on the spot, reduce cost, protect environment is a major issue of giantreed processing technology.
High speed development along with Chinese national economy; The demand of ether of cellulose constantly rises; Be mainly used in industries such as building, papermaking, food, medicine, petrochemical industry; Because the cotton price that production of cellulose ether is used rises steadily, and has caused the continuous increase of ether of cellulose production cost, has increased the weight of the burden of enterprise.
At present production of cellulose ether main raw material still be cotton be main, though the method for patent introduction with wood pulp or bamboo pulp replacement cotton production ether of cellulose arranged, because of severe reaction conditions and the high its intended purposes that do not reach of equipment manufacturing cost.
Summary of the invention
The purpose of this invention is to provide a kind of is the method for feedstock production methyl cellulose ether with the giantreed dissolving pulp, for overcoming the defective of prior art.
Method of the present invention comprises the steps:
(a). giantreed is dissolved starch, and to add volumetric concentration be 75～95% the ethanol and the mixture of sodium hydroxide, 20 ℃-40 ℃ alkalization 2-3 hour, acquisition sodium cellulosate;
The granularity of said giantreed dissolving starch is 200-300 μ m;
The parts by weight of component are:
Volumetric concentration is 100 parts of 75～95% ethanol
20～30 parts of giantreed dissolving starches
10～15 parts in sodium hydroxide
(b). described sodium cellulosate is added etherifying agent, in the presence of combination catalyst, under 45 ℃ of-60 ℃ of temperature etherification reaction 1-2 hour; Then separating reaction liquid with reclaim catalyzer; With 85 ℃-95 ℃ acid solution, soaked 30-60 minute, acid solution is removed in spinning again;
Said acid solution is the acetum of weight concentration 1% or the sulphuric acid soln of weight concentration 0.5%;
Described etherifying agent is a kind of in monochloro methane, methylene dichloride or the trichloromethane or several;
Described combination catalyst comprises following components in weight percentage:
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, said solid super strong alkali preparation method is following:
With 4 gram nitrate of baryta, 4.3 gram Magnesium dichloride hexahydrates and 0.5 gram rubidium nitrate join in 400 milliliters of absolute ethyl alcohols and the 50 milliliters of dioxane mixed solvents ultra-sonic dispersion 30 minutes; Stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 gram Z 150PH, 800 aqueous solution; Continue to stir 4 hours, slowly evaporate whole solvents down at 90 ℃, 500 ℃ of following roastings 2 hours; Obtain solid super base, adopt Chinese patent CN200510011269.0 reported method.
(c.) with the water washing of the product of step b, the centrifugal moisture content of removing with 85 ℃-95 ℃;
(d.) with the product of step c, 90～110 ℃ of dryings, and the control water content is 1-2%, dispersion and fining then, granularity is 60-80 μ m, obtains said methyl cellulose ether;
The working method of described giantreed dissolving pulp comprises the steps;
(1) giantreed is crushed, pulverize segment, length is 3 ~ 5cm;
(2) with the washing of giantreed tablet, remove plaster dirt, the dress pot;
(3) the giantreed sheet is added hydrating solution, in solid acid catalyst, soaked 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 a giantreed tablet;
The parts by weight of said hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2The type solid acid catalyst is made up of the element sulphur of the ZIRCONIUM DIOXIDE 99.5 more than 90% and 0.1～0.5% platinum and 0.5～5%, and median size is 20 nanometers, and through being processed into the agglomeration sphere-like, sphere diameter is 4～6mm usually.
Prepare through following method:
With ZrOCl
2Ammoniacal liquor with 25% in 50 ℃ of following hydrolysis 2 hours (PH is controlled at 10), behind the generation zirconium nitrate, is used 90 ℃ of vaal water soaking and washing 10 hours again; Filter then, clean with 90 ℃ of vaal waters again, after refiltering; 110 ℃ of dryings 10 hours,, soaked 3 hours with being mixed with in 1% dilute sulphuric acid and the 1.67% ammonium chloroplatinate mixed solution again 680 ℃ of following roastings 5 hours; Drying is 3 hours under 110 ℃, again 680 ℃ of following roastings 4 hours, processes solid super-strong acid.(referring to institution of higher education's teaching material " chemical functional materials outline " 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
2The type solid acid catalyst.
(4) then with whole materials of step (3), under 130 ℃-150 ℃ temperature, boiling 30-60 minute;
(5) be warming up to 160 ℃-180 ℃, continue to keep 30-60 minute;
(6) boiling slurry and solid acid catalyst are reclaimed in venting respectively, and the boiling slurry cleans with 80-90 ℃ water;
(7) in the boiling slurry, adding weight concentration is the 5-10% sodium hydroxide solution, soaks 30-60 minute, at 130 ℃ of-150 ℃ of following boiling 30-60 minutes, reclaims 2 times the boiling slurry then;
The weight consumption of said sodium hydroxide solution in sodium hydroxide, is 5～6% of raw material giantreed tablet;
(8) Sulfothiorine and superoxol are added 2 boiling slurries, add water to slurry again and flood, feed steam, be warming up to 90 ℃-120 ℃, bleached 30-60 minute, reclaim the 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 is used to prepare ether of cellulose or paper making raw material.
The invention has the advantages that and utilized resourceful giantreed to be raw material, become dissolving pulp through giantreed production preliminary working, 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 reduced the temperature of etherification reaction but also shortened time of etherification reaction, reduced corrosion in process of production production unit; Reduced energy consumption; Significantly reduce the waste liquid that produces in the production process, improved effective utilization, protection environment particular significant effect water resources.The present invention invests little, and technology 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, the giantreed dissolving pulp is produced the method for methyl cellulose ether:
(a). in 100 parts of 95% ethanol, 10 parts in sodium hydroxide, heating makes dissolution of sodium hydroxide, adds 20 parts of giantreed dissolving starches, stirs alkalization 3 hours at 20 ℃, makes it to generate sodium cellulosate.
The granularity of giantreed dissolving starch is 200 μ m;
The parts by weight of component are:
Volumetric concentration is 100 parts of 95% ethanol
20 parts of giantreed dissolving starches
10 parts in sodium hydroxide
(b). with adding etherifying agent in the described sodium cellulosate; In the presence of combination catalyst; Etherification reaction is 2 hours under 45 ℃ of temperature; Then separating reaction liquid with reclaim combination catalyst, the weight concentration of using 95 ℃ is 100 parts of immersions of acetum of 1% 30 minutes, removes acid solution with whizzer again;
Described etherifying agent is a 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 coats with 300 purpose stainless (steel) wires.
The preparation method of solid super base: with 4 gram nitrate of baryta, 4.3 gram Magnesium dichloride hexahydrates and 0.5 gram rubidium nitrate join in 400 milliliters of absolute ethyl alcohols and the 50 milliliters of dioxane mixed solvents ultra-sonic dispersion 30 minutes; Stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 gram Z 150PH, 800 aqueous solution; Continue to stir 4 hours, slowly evaporate whole solvents down at 90 ℃, 500 ℃ of following roastings 2 hours; Obtain solid super base, adopt Chinese patent CN200510011269.0 reported method.
The particle diameter of nanometer cuprous chloride, nano silver/silver chloride is 20～40 nanometers; Preferred 30 nanometers.
(c.) clean the remaining acid solution in ether of cellulose surface with 95 ℃ of vaal waters, then with the centrifugal moisture content of removing of whizzer;
(d) product with step c carries out drying under 90 ℃, control water content be 1%, again with kibbler with the ether of cellulose refinement, control average particle size be 60 μ m, obtain described methyl cellulose ether.
Two, the working method of giantreed dissolving pulp:
(a) giantreed is crushed, pulverize segment, mean length is 3cm;
(b) with the washing of giantreed tablet, remove plaster dirt, the dress pot;
(c) the giantreed sheet is added hydrating solution, in solid acid catalyst, soaked 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 a giantreed tablet;
The parts by weight of said hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2The type solid acid catalyst is made up of the element sulphur of the ZIRCONIUM DIOXIDE 99.5 more than 90% and 0.1～0.5% platinum and 0.5～5%, and median size is 20 nanometers, and through being processed into the agglomeration sphere-like, sphere diameter is 4～6mm usually.
Prepare through following method:
With ZrOCl
2Ammoniacal liquor with 25% in 50 ℃ of following hydrolysis 2 hours (PH is controlled at 10), behind the generation zirconium nitrate, is used 90 ℃ of vaal water soaking and washing 10 hours again; Filter then, clean with 90 ℃ of vaal waters again, after refiltering; 110 ℃ of dryings 10 hours,, soaked 3 hours with being mixed with in 1% dilute sulphuric acid and the 1.67% ammonium chloroplatinate mixed solution again 680 ℃ of following roastings 5 hours; Drying is 3 hours under 110 ℃, again 680 ℃ of following roastings 4 hours, processes solid super-strong acid.
(d) then with whole materials of step (3), under 130 ℃, boiling 30 minutes;
(e) being warming up to 160 ℃ continues down to keep 30 minutes;
(f) boiling slurry and solid acid catalyst are reclaimed in venting respectively, and the boiling slurry cleans with 80 ℃ water;
(g) in the boiling slurry, adding weight concentration is 5% sodium hydroxide solution, soaks 30 minutes, and under 130 ℃, the boiling slurry is reclaimed 2 times in boiling 30 minutes then;
The weight consumption of sodium hydroxide solution in sodium hydroxide, is 5% of raw material giantreed tablet;
(h) Sulfothiorine and superoxol are added 2 boiling slurries, add water to slurry again and flood, feed steam, be warming up to 90 ℃, bleached 30 minutes, reclaim the bleaching slurry; Giantreed dissolving pulp for preliminary working is used to prepare 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, the giantreed dissolving pulp is produced the method for methyl cellulose ether:
(a). in 100 parts of 85% ethanol, 15 parts in sodium hydroxide, heating makes dissolution of sodium hydroxide, adds 30 parts of giantreed dissolving starches, stirs alkalization 2 hours at 40 ℃, makes it to generate sodium cellulosate.
The granularity of giantreed dissolving 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 in sodium hydroxide
(b). described sodium cellulosate is added etherifying agent; In the presence of the catalyzer of combination, etherification reaction is 1 hour under 45 ℃ of ℃ of temperature, then separating reaction liquid and recovery combination catalyst; The weight concentration of using 95 ℃ is that 0.5% sulphuric acid soln soaked 60 minutes for 100 parts, removes acid solution with whizzer again;
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 coats with 300 purpose stainless (steel) wires.
The preparation method of solid super base: with 4 gram nitrate of baryta, 4.3 gram Magnesium dichloride hexahydrates and 0.5 gram rubidium nitrate join in 400 milliliters of absolute ethyl alcohols and the 50 milliliters of dioxane mixed solvents ultra-sonic dispersion 30 minutes; Stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 gram Z 150PH, 800 aqueous solution; Continue to stir 4 hours, slowly evaporate whole solvents down at 90 ℃, 500 ℃ of following roastings 2 hours; Obtain solid super base, adopt Chinese patent CN200510011269.0 reported method.
The particle diameter of nanometer cuprous chloride, nano silver/silver chloride is 20 nanometers.
(c). clean the remaining acid solution in ether of cellulose surface with 85 ℃ of vaal waters; Then with the centrifugal moisture content of removing of whizzer; (d) product with step c carries out drying under 100 ℃, control water content be 2%, again with kibbler with the ether of cellulose refinement; The control average particle size is 80 μ m, is product.
Two, the working method of giantreed dissolving pulp:
(a) giantreed is crushed, pulverize segment, mean length is 5cm;
(b) with the washing of giantreed tablet, remove plaster dirt, the dress pot;
(c) the giantreed sheet is added hydrating solution, in solid acid catalyst, soaked 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 a giantreed tablet;
The parts by weight of said hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2The type solid acid catalyst is made up of the element sulphur of the ZIRCONIUM DIOXIDE 99.5 more than 90% and 0.1～0.5% platinum and 0.5～5%, and median size is 20 nanometers, and through being processed into the agglomeration sphere-like, sphere diameter is 4～6mm usually.
Prepare through following method:
With ZrOCl
2Ammoniacal liquor with 25% in 50 ℃ of following hydrolysis 2 hours (PH is controlled at 10), behind the generation zirconium nitrate, is used 90 ℃ of vaal water soaking and washing 10 hours again; Filter then, again with 90 ℃ of vaal waters cleanings, after refiltering, 110 ℃ of dryings 10 hours; 680 ℃ of following roastings 5 hours, soaked 3 hours with being mixed with in 1% dilute sulphuric acid and the 1.67% ammonium chloroplatinate mixed solution again, after refiltering; Drying is 3 hours under 110 ℃, again 680 ℃ of following roastings 4 hours, processes solid super-strong acid.
(d) then with whole materials of step (3), under 150 ℃, boiling 60 minutes;
(e) be warming up to 180 ℃, continue to keep 60 minutes;
(f) boiling slurry and solid acid catalyst are reclaimed in venting respectively, and the boiling slurry cleans with 80-90 ℃ water;
(g) in the boiling slurry, adding weight concentration is 10% sodium hydroxide solution, soaks 60 minutes, and 150 ℃ then, the boiling slurry is reclaimed 2 times in boiling 30 minutes;
The weight consumption of sodium hydroxide solution in sodium hydroxide, is 6% of raw material giantreed tablet;
(h) Sulfothiorine and superoxol are added 2 boiling slurries, add water to slurry again and flood, feed steam, be warming up to 120 ℃, bleached 60 minutes, reclaim the 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, the giantreed dissolving pulp is produced the method for methyl cellulose ether, by following steps:
(a). in 100 parts of 75% ethanol, 12.5 parts in sodium hydroxide, heating makes dissolution of sodium hydroxide, adds 25 parts of giantreed dissolving starches, stirs alkalization 2.5 hours at 30 ℃, makes it to generate sodium cellulosate.
The granularity of giantreed dissolving starch is 250 μ m;
The parts by weight of component are:
Volumetric concentration is 100 parts of 75% ethanol
25 parts of giantreed dissolving starches
12.5 parts in sodium hydroxide
(b). described sodium cellulosate is added etherifying agent; In the presence of the catalyzer of combination, etherification reaction is 2 hours under 45 ℃ of temperature, then separating reaction liquid and recovery combination catalyst; The weight concentration of using 95 ℃ is that 1% acetum soaked 45 minutes for 100 parts, removes acid solution with whizzer again;
Described etherifying agent is a trichloromethane;
Combination catalyst component: 99% solid super base, 0.5% nanometer cuprous chloride, 0.5% nano silver/silver chloride; Catalyzer coats with 300 purpose stainless (steel) wires.
The preparation method of solid super base: with 4 gram nitrate of baryta, 4.3 gram Magnesium dichloride hexahydrates and 0.5 gram rubidium nitrate join in 400 milliliters of absolute ethyl alcohols and the 50 milliliters of dioxane mixed solvents ultra-sonic dispersion 30 minutes; Stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 gram Z 150PH, 800 aqueous solution; Continue to stir 4 hours, slowly evaporate whole solvents down at 90 ℃, 500 ℃ of following roastings 2 hours; Obtain solid super base, adopt Chinese patent CN200510011269.0 reported method.
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 vaal waters, then with the centrifugal moisture content of removing of whizzer,
The product that ﹙ d ﹚ gathers the step c carries out drying under 110 ℃, the control water content is 1-2%, again with kibbler with the ether of cellulose refinement, control average particle size be 80 μ m, be product.
Two, the working method of giantreed dissolving pulp
(a) giantreed is crushed, pulverize segment, mean length is 4cm;
(b) with the washing of giantreed tablet, remove plaster dirt, the dress pot;
(c) the giantreed sheet is added hydrating solution, in solid acid catalyst, soaked 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 a giantreed tablet;
The parts by weight of said hydrating solution comprise:
Described solid acid catalyst is SO
4 2--ZrO
2The type solid acid catalyst is made up of the element sulphur of the ZIRCONIUM DIOXIDE 99.5 more than 90% and 0.1～0.5% platinum and 0.5～5%, and median size is 20 nanometers, and through being processed into the agglomeration sphere-like, sphere diameter is 4～6mm usually.
Prepare through following method:
With ZrOCl
2Ammoniacal liquor with 25% in 50 ℃ of following hydrolysis 2 hours (PH is controlled at 10), behind the generation zirconium nitrate, is used 90 ℃ of vaal water soaking and washing 10 hours again; Filter then, clean with 90 ℃ of vaal waters again, after refiltering; 110 ℃ of dryings 10 hours,, soaked 3 hours with being mixed with in 1% dilute sulphuric acid and the 1.67% ammonium chloroplatinate mixed solution again 680 ℃ of following roastings 5 hours; Drying is 3 hours under 110 ℃, again 680 ℃ of following roastings 4 hours, processes solid super-strong acid.
(d) then with whole materials (comprising giantreed tablet, hydrating solution and solid acid catalyst) of step (3), under 140 ℃, boiling 45 minutes;
(e) being warming up to 170 ℃ continues down to keep 50 minutes;
(f) boiling slurry and solid acid catalyst are reclaimed in venting respectively, and the boiling slurry cleans with 80-90 ℃ water;
(g) in the boiling slurry, adding weight concentration is 8% sodium hydroxide solution, soaks 45 minutes, and 140 ℃ then, the boiling slurry is reclaimed 2 times in boiling 45 minutes;
The weight consumption of sodium hydroxide solution in sodium hydroxide, is 5.5% of raw material giantreed tablet;
(h) Sulfothiorine and superoxol are added 2 boiling slurries, add water to slurry again and flood, feed steam, be warming up to 105 ℃, bleached 45 minutes, reclaim the 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, the giantreed dissolving pulp is produced the method for methyl cellulose ether:
(a). in 100 parts of 90% ethanol, 15 parts in sodium hydroxide, heating makes dissolution of sodium hydroxide, adds 30 parts of giantreed dissolving starches, stirs alkalization 2 hours at 40 ℃, makes it to generate sodium cellulosate.
The granularity of giantreed dissolving 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 starches
15 parts in sodium hydroxide
(b). described sodium cellulosate is added etherifying agent; In the presence of the catalyzer of combination, etherification reaction is 1 hour under 45 ℃ of temperature, then separating reaction liquid and recovery combination catalyst; Using 95 ℃ of weight concentrations is that 0.5% sulphuric acid soln soaked 60 minutes for 100 parts, removes acid solution with whizzer again;
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 coats with 300 purpose stainless (steel) wires.
The preparation method of solid super base: with 4 gram nitrate of baryta, 4.3 gram Magnesium dichloride hexahydrates and 0.5 gram rubidium nitrate join in 400 milliliters of absolute ethyl alcohols and the 50 milliliters of dioxane mixed solvents ultra-sonic dispersion 30 minutes; Stirring is warmed up to 70 ℃ and slowly drips 400 milliliters of 7 gram Z 150PH, 800 aqueous solution; Continue to stir 4 hours, slowly evaporate whole solvents down at 90 ℃, 500 ℃ of following roastings 2 hours; Obtain solid super base, adopt Chinese patent CN200510011269.0 reported method.
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 vaal waters, then with the centrifugal moisture content of removing of whizzer,
The product that ﹙ d ﹚ rises step c carries out drying under 100 ℃, the control water content is 1-2%, again with kibbler with the ether of cellulose refinement, control average particle size at 70 μ m.
Two, the working method of giantreed dissolving pulp is with embodiment 1.
The mensuration of embodiment ether of cellulose is following:
The effect of embodiment ether of cellulose in sand-cement slurry: reference standard JC/T992-2006
Judge that from the effect sand-cement slurry methyl cellulose ether of the present invention reaches the effect with the ether of cellulose of cotton production fully.
Claims (3)
1. be the method for feedstock production methyl cellulose ether with the giantreed dissolving pulp, it is characterized in that, comprise the steps:
(a). giantreed is dissolved the mixture that starch adds ethanol and sodium hydroxide, and alkalization obtains sodium cellulosate;
(b). described sodium cellulosate is added etherifying agent, and in the presence of combination catalyst, etherification reaction is collected reaction solution then, soaks with acid solution, and acid solution is removed in spinning;
(c.) product of step b is used water washing, remove moisture content;
(d.) with the product of step c, drying, dispersion and fining obtains said methyl cellulose ether then.
2. method according to claim 1 is characterized in that, in the step (a), the parts by weight of component are:
Volumetric concentration is 100 parts of 75～95% ethanol
20～30 parts of giantreed dissolving starches
10～15 parts in sodium hydroxide.
3. method according to claim 1 and 2 is characterized in that, in the step (b); Described sodium cellulosate is added etherifying agent; In the presence of combination catalyst, under 45 ℃ of-60 ℃ of temperature etherification reaction 1-2 hour, collect reaction solution then; Soaked 30-60 minute with 85 ℃-95 ℃ acid solutions, acid solution is removed in spinning;
The parts by weight of each component are:
Said acid solution is that acetum or the weight concentration of weight concentration 1% is 0.5% sulphuric acid soln;
Described etherifying agent is a kind of in monochloro methane, methylene dichloride or the trichloromethane or several;
Described combination catalyst comprises following components in weight percentage:
Solid super base 98～99%
Nanometer cuprous chloride 0.5～1%
Nano silver/silver chloride 0.5～1%.
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Cited By (5)
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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 |
| CN103483456A (en) * | 2013-10-15 | 2014-01-01 | 湖北博斐逊生物新材料有限公司 | Preparation method of cement sizing fiber and application thereof in cement products |
| 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 |
| 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 |
| CN111344309A (en) * | 2017-10-03 | 2020-06-26 | 陶氏环球技术有限责任公司 | Simplified process for making low viscosity cellulose ethers |
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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 |
| CN103483456A (en) * | 2013-10-15 | 2014-01-01 | 湖北博斐逊生物新材料有限公司 | Preparation method of cement sizing fiber and application thereof in cement products |
| 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 |
| CN111344309A (en) * | 2017-10-03 | 2020-06-26 | 陶氏环球技术有限责任公司 | Simplified process for making low viscosity cellulose ethers |
| CN111344309B (en) * | 2017-10-03 | 2022-04-19 | 陶氏环球技术有限责任公司 | Simplified process for making low viscosity cellulose ethers |
| 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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