CN102219863A - Process for modifying hydroxyethylcellulose (HEC) by high-carbon alkylation - Google Patents
Process for modifying hydroxyethylcellulose (HEC) by high-carbon alkylation Download PDFInfo
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Abstract
The invention discloses a process for modifying hydroxyethylcellulose (HEC) by high-carbon alkylation, and relates to the field of fine chemical engineering. The hydroxyethylcellulose (HEC) is modified by high-carbon alkyl, so that the stability of the hydroxyethylcellulose (HEC) in application of emulsion paint is improved greatly, construction splatter is reduced, the fungus resistance of products can be improved by 20 to 30 percent, the shelf life of the produced emulsion paint is prolonged by 3 to 5 months, and the using effect of the hydroxyethylcellulose (HEC) in the emulsion paint can completely reach the same level in foreign countries. Due to the adoption of a computer control technology, the labor intensity of workers is reduced, labor is reduced, and the labor efficiency and production safety are improved.
Description
Technical field
The present invention relates to field of fine chemical, the technology of specifically a kind of high-carbon alkylation modification Natvosol (HEC).
Background technology
Natvosol (HEC) is to use natural cellulose under the effect of solvent and alkali, make with reacting ethylene oxide, at present, Natvosol (HEC) substitution value that domestic most of enterprise produces generally can only reach 1.5-2.0, the effect of product in emulsion paint is bad, the stability in storage of emulsion paint is low, is easy to generate in the brushing process of emulsion paint and splashes, 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 the technology of a kind of high-carbon alkylation modification Natvosol (HEC), utilize the residual hydroxyl in high-carbon moieties replacement Natvosol (HEC) structure, improve the degree of uniformity that polymer replaces, improve the stability of product.
For achieving the above object, the technical solution used in the present invention is as follows:
The technology of a kind of high-carbon alkylation modification Natvosol (HEC), realized by following step:
1) pulverize: the refined cellulose of getting 1000 mass parts is pulverized, is separated, and reaches about 80 orders of 0.03-0.15mm(), tails dedusting;
2) alkalization: in reactor, add the alcoholic solution of 5000-12000 mass parts, stir, add the sheet alkali of 200-280 mass parts, be warmed up to 50-70 ℃ of choline, cooling to normal temperature after choline finishes, add above-mentioned refined cellulose, is alkalization 0.5-1.5 hour under 15-35 ℃ the situation in temperature;
3) reaction: the high-carbon alkyl bromide that in reactor, adds the 10-50 mass parts, stirred 30-60 minute, the oxyethane that adds the 900-1300 mass parts then, reaction process is divided two stages, fs is to be reaction 0.5-3.5 hour under 50-60 ℃ the situation in temperature, subordinate phase is to be reaction 0.5-4 hour under 65-80 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the acid solution of 300-500 mass parts is 5.5-8.5 under 40-60 ℃ the situation in temperature, in the time be 0.5-1 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, and solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1-2 hour under 20-35 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Described alcoholic solution can be Virahol, n-propyl alcohol, isopropylcarbinol, propyl carbinol.
Described acid solution can be hydrochloric acid, oxalic acid, acetic acid, phosphoric acid.
Described high-carbon alkyl bromide can be lauryl bromide, tetradecyl bromine, hexadecyl bromine.
The present invention adopts the high-carbon alkyl to come modified hydroxyethylcellulosadsorbing (HEC), improved the stability of its Natvosol (HEC) in emulsion paint is used greatly, having reduced construction splashes, the midew proof of its product can improve 20%-30%, the emulsion paint shelf life extension 3-5 that produces month, the result of use in emulsion paint can reach external peer-level fully; Adopt Computer Control Technology, reduced intensity of workers, reduced simultaneously manually, improved efficiency and production security.
Description of drawings
Accompanying drawing is a process 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 natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: add the aqueous isopropanol of 5000 mass parts in reactor, stir, add the sheet alkali of 280 mass parts, be warmed up to 50 ℃ of cholines, choline cools to normal temperature after finishing, and adds above-mentioned refined cellulose, is alkalization 0.5 hour under 35 ℃ the situation in temperature;
3) reaction: the lauryl bromide that in reactor, adds 50 mass parts, stirred 30 minutes, the oxyethane that adds 1300 mass parts then, reaction process is divided two stages, fs is to be reaction 1.5 hours under 50 ℃ the situation in temperature, subordinate phase is to be reaction 3 hours under 65 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the acetum of 500 mass parts is 5.5 under 40 ℃ the situation in temperature, in the time be 1 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 2 hours under 20 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 2:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: add the n-propyl alcohol solution of 10000 mass parts in reactor, stir, add the sheet alkali of 250 mass parts, be warmed up to 60 ℃ of cholines, choline cools to normal temperature after finishing, and adds above-mentioned refined cellulose, is alkalization 1 hour under 20 ℃ the situation in temperature;
3) reaction: the lauryl bromide that in reactor, adds 30 mass parts, stirred 40 minutes, the oxyethane that adds 1000 mass parts then, reaction process is divided two stages, fs is to be reaction 1 hour under 55 ℃ the situation in temperature, subordinate phase is to be reaction 2.5 hours under 70 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the acetum of 400 mass parts is 7 under 50 ℃ the situation in temperature, in the time be 0.6 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1.5 hours under 30 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 3:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: add the butanol solution of 6000 mass parts in reactor, stir, add the sheet alkali of 240 mass parts, be warmed up to 65 ℃ of cholines, choline cools to normal temperature after finishing, and adds above-mentioned refined cellulose, is alkalization 0.8 hour under 25 ℃ the situation in temperature;
3) reaction: the tetradecyl bromine that in reactor, adds 20 mass parts, stirred 50 minutes, the oxyethane that adds 1200 mass parts then, reaction process is divided two stages, fs is to be reaction 0.6 hour under 60 ℃ the situation in temperature, subordinate phase is to be reaction 0.6 hour under 75 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the oxalic acid solution of 450 mass parts is 7.5 under 45 ℃ the situation in temperature, in the time be 0.8 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1.2 hours under 25 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 4:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: in reactor, add the aqueous isopropanol of 12000 mass parts, stir, add the sheet alkali of 200 mass parts, be warmed up to 70 ℃ of cholines, cooling to normal temperature after choline finishes, add above-mentioned refined cellulose, is alkalization 1.5 hours under 15 ℃ the situation in temperature;
3) reaction: the tetradecyl bromine that in reactor, adds 10 mass parts, stirred 60 minutes, the oxyethane that adds 900 mass parts then, reaction process is divided two stages, fs is to be reaction 0.5 hour under 60 ℃ the situation in temperature, subordinate phase is to be reaction 0.5 hour under 80 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the phosphoric acid solution of 300 mass parts is 8.5 under 60 ℃ the situation in temperature, in the time be 0.5 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1 hour under 35 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 5:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: add the isobutanol solution of 10000 mass parts in reactor, stir, add the sheet alkali of 250 mass parts, be warmed up to 70 ℃ of cholines, choline cools to normal temperature after finishing, and adds above-mentioned refined cellulose, is alkalization 1 hour under 35 ℃ the situation in temperature;
3) reaction: the hexadecyl bromine that in reactor, adds 40 mass parts, stirred 35 minutes, the oxyethane that adds 1000 mass parts then, reaction process is divided two stages, fs is to be reaction 1 hour under 55 ℃ the situation in temperature, subordinate phase is to be reaction 2.5 hours under 70 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the acetum of 400 mass parts is 7 under 50 ℃ the situation in temperature, in the time be 0.6 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1.5 hours under 30 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 6:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: add the aqueous isopropanol of 8000 mass parts in reactor, stir, add the sheet alkali of 260 mass parts, be warmed up to 55 ℃ of cholines, choline cools to normal temperature after finishing, and adds above-mentioned refined cellulose, is alkalization 0.6 hour under 30 ℃ the situation in temperature;
3) reaction: the tetradecyl bromine that in reactor, adds 35 mass parts, stirred 45 minutes, the oxyethane that adds 1000 mass parts then, reaction process is divided two stages, fs is to be reaction 1.5 hours under 50 ℃ the situation in temperature, subordinate phase is to react 2.0 hours under the situation of 80 ℃ of temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the hydrochloric acid soln of 350 mass parts is 8 under 50 ℃ the situation in temperature, in the time be 0.8 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1 hour under 35 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 7:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: add the n-propyl alcohol solution of 9000 mass parts in reactor, stir, add the sheet alkali of 280 mass parts, be warmed up to 60 ℃ of cholines, choline cools to normal temperature after finishing, and adds above-mentioned refined cellulose, is alkalization 0.8 hour under 25 ℃ the situation in temperature;
3) reaction: the hexadecyl bromine that in reactor, adds 20 mass parts, stirred 60 minutes, the oxyethane that adds 1000 mass parts then, reaction process is divided two stages, fs is to be reaction 1.2 hours under 60 ℃ the situation in temperature, subordinate phase is to be reaction 1.5 hours under 70 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the acetum of 400 mass parts is 8.5 under 60 ℃ the situation in temperature, in the time be 1 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 2 hours under 20 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 8:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: add the aqueous isopropanol of 5000 mass parts in reactor, stir, add the sheet alkali of 250 mass parts, be warmed up to 60 ℃ of cholines, choline cools to normal temperature after finishing, and adds above-mentioned refined cellulose, is alkalization 1 hour under 30 ℃ the situation in temperature;
3) reaction: the tetradecyl bromine that in reactor, adds 40 mass parts, stirred 40 minutes, the oxyethane that adds 1000 mass parts then, reaction process is divided two stages, fs is to be reaction 1 hour under 55 ℃ the situation in temperature, subordinate phase is to be reaction 4 hours under 70 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the oxalic acid solution of 400 mass parts is 6 under 40 ℃ the situation in temperature, in the time be 0.8 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1.5 hours under 30 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 9:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: in reactor, add the isobutanol solution of 10000 mass parts, stir, add the sheet alkali of 280 mass parts, be warmed up to 70 ℃ of cholines, cooling to normal temperature after choline finishes, add above-mentioned refined cellulose, is alkalization 0.5 hour under 15 ℃ the situation in temperature;
3) reaction: the lauryl bromide that in reactor, adds 50 mass parts, stirred 30 minutes, the oxyethane that adds 1000 mass parts then, reaction process is divided two stages, fs is to be reaction 3.5 hours under 50 ℃ the situation in temperature, subordinate phase is to be reaction 0.8 hour under 65 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the phosphoric acid solution of 400 mass parts is 7 under 50 ℃ the situation in temperature, in the time be 0.6 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1.5 hours under 30 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
Embodiment 10:
1) pulverize: the natural refined cellulose that will become bag is got 1000 mass parts through opening bag, pulverizes with rotating knife formula pulverizer, separates through cyclonic separator, reaches about 80 orders of 0.03-0.15mm(), tail gas is through bag-type dusting;
2) alkalization: add the aqueous isopropanol of 10000 mass parts in reactor, stir, add the sheet alkali of 200 mass parts, be warmed up to 65 ℃ of cholines, choline cools to normal temperature after finishing, and adds above-mentioned refined cellulose, is alkalization 1 hour under 20 ℃ the situation in temperature;
3) reaction: the hexadecyl bromine that in reactor, adds 40 mass parts, stirred 40 minutes, the oxyethane that adds 1200 mass parts then, reaction process is divided two stages, fs is to be reaction 1 hour under 50 ℃ the situation in temperature, subordinate phase is to be reaction 0.8 hour under 70 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the acetum of 450 mass parts is 7 under 45 ℃ the situation in temperature, in the time be 0.6 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, use the spiral pump convey materials, separate with the horizontal spiral separating machine, solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1.5 hours under 30 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, uses the spiral pump convey materials, separates with the horizontal spiral separating machine, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles.
8) drying, packing.
The leading indicator that product reaches:
Total substitution value: 1.8-2.5 improves 10-20% 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) 10000-100000mPa.s.
Claims (4)
1. the technology of a high-carbon alkylation modification Natvosol (HEC) is characterized in that, is realized by following step:
1) pulverize: the refined cellulose of getting 1000 mass parts is pulverized, is separated, and reaches about 80 orders of 0.03-0.15mm(), tails dedusting;
2) alkalization: in reactor, add the alcoholic solution of 5000-12000 mass parts, stir, add the sheet alkali of 200-280 mass parts, be warmed up to 50-70 ℃ of choline, cooling to normal temperature after choline finishes, add above-mentioned refined cellulose, is alkalization 0.5-1.5 hour under 15-35 ℃ the situation in temperature;
3) reaction: the high-carbon alkyl bromide that in reactor, adds the 10-50 mass parts, stirred 30-60 minute, the oxyethane that adds the 900-1300 mass parts then, reaction process is divided two stages, fs is to be reaction 0.5-3.5 hour under 50-60 ℃ the situation in temperature, subordinate phase is to be reaction 0.5-4 hour under 65-80 ℃ the situation in temperature, and reaction process is carried out time variable control by computer;
4) neutralization: be that the pH value of adjusting above-mentioned gained solution with the acid solution of 300-500 mass parts is 5.5-8.5 under 40-60 ℃ the situation in temperature, in the time be 0.5-1 hour;
5) flash liberation: gained solution in the aforesaid reaction vessel is carried out flash liberation, and solid materials enters the washing still, and evaporation enters reactor to liquid solvent through the solvent evaporation device, recycles;
6) washing: in the washing still, the fixedly material in the step 5) is washing 1-2 hour under 20-35 ℃ the situation in temperature;
7) secondary separation: the solution that will wash in the still carries out secondary separation, and solid materials enters the washing still, and evaporation enters the washing still to liquid solvent through the solvent evaporation device, recycles;
8) drying, packing.
2. the technology of high-carbon alkylation modification Natvosol according to claim 1 (HEC) is characterized in that, described alcoholic solution can be Virahol, n-propyl alcohol, isopropylcarbinol, propyl carbinol.
3. the technology of high-carbon alkylation modification Natvosol according to claim 1 (HEC) is characterized in that, described acid solution can be hydrochloric acid, oxalic acid, acetic acid, phosphoric acid.
4. the technology of high-carbon alkylation modification Natvosol according to claim 1 (HEC) is characterized in that, described high-carbon alkyl bromide can be lauryl bromide, tetradecyl bromine, hexadecyl bromine.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107266703A (en) * | 2017-05-25 | 2017-10-20 | 华南理工大学 | A kind of method using the materials of micro-diplopore HKUST 1 in neutral template normal temperature synthesis lamella |
CN107814847A (en) * | 2016-09-12 | 2018-03-20 | 中国石油化工股份有限公司 | A kind of hydrophobically modified hydroxyethyl cellulose fluid loss agent, preparation method and characterizing method |
CN107964048A (en) * | 2018-01-04 | 2018-04-27 | 泸州北方化学工业有限公司 | A kind of coating process of hydrophobic associated ethoxyl cellulose |
CN115716881A (en) * | 2022-11-28 | 2023-02-28 | 泸州北方纤维素有限公司 | Hydrophobically modified hydroxyethyl cellulose and preparation method thereof |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1032796A (en) * | 1987-09-17 | 1989-05-10 | 阿奎龙公司 | Natvosol of carboxymethyl hydrophobically modified (CMHMHEC) and the application in protective coating compositions thereof |
EP0566911A1 (en) * | 1992-04-20 | 1993-10-27 | Aqualon Company | Improved leveling aqueous coating compositions |
US20020038018A1 (en) * | 2000-08-10 | 2002-03-28 | Wolfgang Dannhorn | Process for preparing alkylhydroxyalkyl cellulose |
US20030226213A1 (en) * | 2002-04-16 | 2003-12-11 | The Procter & Gamble Company | Textile mill applications of cellulosic based polymers to provide appearance and integrity benefits to fabrics during laundering and in-wear |
US20040127700A1 (en) * | 2002-07-25 | 2004-07-01 | Hartwig Schlesiger | Cellulose derivatives having gel-like rheological properties and process for the preparation thereof |
CN101177261A (en) * | 2007-11-08 | 2008-05-14 | 上海交通大学 | Method for preparing biocompatible cellulose functionalized carbon nano tube |
-
2011
- 2011-05-06 CN CN201110116638A patent/CN102219863B/en not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1032796A (en) * | 1987-09-17 | 1989-05-10 | 阿奎龙公司 | Natvosol of carboxymethyl hydrophobically modified (CMHMHEC) and the application in protective coating compositions thereof |
EP0566911A1 (en) * | 1992-04-20 | 1993-10-27 | Aqualon Company | Improved leveling aqueous coating compositions |
US20020038018A1 (en) * | 2000-08-10 | 2002-03-28 | Wolfgang Dannhorn | Process for preparing alkylhydroxyalkyl cellulose |
US20030226213A1 (en) * | 2002-04-16 | 2003-12-11 | The Procter & Gamble Company | Textile mill applications of cellulosic based polymers to provide appearance and integrity benefits to fabrics during laundering and in-wear |
US20040127700A1 (en) * | 2002-07-25 | 2004-07-01 | Hartwig Schlesiger | Cellulose derivatives having gel-like rheological properties and process for the preparation thereof |
CN101177261A (en) * | 2007-11-08 | 2008-05-14 | 上海交通大学 | Method for preparing biocompatible cellulose functionalized carbon nano tube |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107814847A (en) * | 2016-09-12 | 2018-03-20 | 中国石油化工股份有限公司 | A kind of hydrophobically modified hydroxyethyl cellulose fluid loss agent, preparation method and characterizing method |
CN107814847B (en) * | 2016-09-12 | 2020-06-09 | 中国石油化工股份有限公司 | Hydrophobically modified hydroxyethyl cellulose fluid loss agent, preparation method and characterization method |
CN107266703A (en) * | 2017-05-25 | 2017-10-20 | 华南理工大学 | A kind of method using the materials of micro-diplopore HKUST 1 in neutral template normal temperature synthesis lamella |
CN107964048A (en) * | 2018-01-04 | 2018-04-27 | 泸州北方化学工业有限公司 | A kind of coating process of hydrophobic associated ethoxyl cellulose |
CN115716881A (en) * | 2022-11-28 | 2023-02-28 | 泸州北方纤维素有限公司 | Hydrophobically modified hydroxyethyl cellulose and preparation method thereof |
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