CN101435115A - Preparation technique of cellulose fibre spinning solution - Google Patents
Preparation technique of cellulose fibre spinning solution Download PDFInfo
- Publication number
- CN101435115A CN101435115A CNA200810238473XA CN200810238473A CN101435115A CN 101435115 A CN101435115 A CN 101435115A CN A200810238473X A CNA200810238473X A CN A200810238473XA CN 200810238473 A CN200810238473 A CN 200810238473A CN 101435115 A CN101435115 A CN 101435115A
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- CN
- China
- Prior art keywords
- cellulose
- spinning solution
- urea
- alkali
- preparation technology
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000009987 spinning Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000004202 carbamide Substances 0.000 claims abstract description 30
- 239000003513 alkali Substances 0.000 claims abstract description 29
- 229920002678 cellulose Polymers 0.000 claims abstract description 27
- 239000001913 cellulose Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 238000005516 engineering process Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract 2
- 229920000742 Cotton Polymers 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229920001131 Pulp (paper) Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 8
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- 238000007598 dipping method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation technology of cellulose fiber spinning solution. Cellulose pulp is adopted, subjected to alkalization, squeezing, crushing, and cooling to room temperature, mixed with urea aqueous solution, cooled to minus 5 DEG C to 15 DEG C, and stirred till alkali cellulose completely dissolves, and vacuum defoamation is carried out simultaneously in dissolution to prepare the uniform and transparent spinning solution. The solution has good spinning performance.
Description
Technical field
The present invention relates to a kind of spinning solution preparation technology of solvent spun fibre.
Background technology
For a long time, the relative contradiction that falls behind with production Technology of the market demand of regenerated celulose fibre becomes the bottleneck that regenerated celulose fibre further expands.Along with the raising of environmental protection consciousness in the worldwide, this contradiction is outstanding day by day, seeks the novel solvent of regenerated celulose fibre green processing, and the new way that solves this contradiction is provided.But domestic viscose production clean production, the progress of especially industrialization aspect does not satisfy the needs of enterprise development far away.At present, the amine oxide system (NMMO) that has made substantial progress, ion liquid system solvent can't be born the important task of viscose glue industry revolution rapidly in a short time also because of bottleneck problems such as expensive raw material price, recovery difficult are big, titles to patent.
Urea/buck system is a kind of cellulosic new class solvent of up-to-date exploitation, it is cheap and easy to get that this system solvent has raw material, technology is simple, characteristics such as the easy recovery of chemical raw material, but the method for the present employed urea of people/buck system dissolving cellulos, or cellulosic solubility is low, have only about 5%, or adopt cellulose is mixed back precooling generation alkali cellulose with sodium hydrate aqueous solution, mix with urea again, cellulose alkalization under the precooling situation, cellulose swollen in alkali lye is very violent, and further dissolving will have very high requirement to equipment.
Summary of the invention
The invention provides a kind of urea/buck system that adopts is the preparation technology of the cellulose fibre spinning solution of solvent production.
The preparation technology of this cellulose fibre spinning solution is for being raw material with the cellulose slurry, make alkali cellulose through alkalization, squeezing with after pulverizing, be cooled to room temperature 10-30 ℃, mix with aqueous solution of urea, can adopt in reactor and mix, be cooled to-5 ℃ then with aqueous solution of urea---after 15 ℃, be stirred to alkali cellulose and dissolve fully, in dissolving, carry out vacuum defoamation, make homogeneous, transparent spinning solution.
Wherein used pulp is that the degree of polymerization is cotton pulp or the wood pulp of 300-500.
Described alkalization temperature is 40-60 ℃, and alkali is dense to be 80-250g/L, and alkalization time is 5-50 minute;
The described alkali cellulose cellulose quality content that makes is 10-40%, and the alkali mass content is 5-20%.
Urea quality content is 5%-15% in the described aqueous solution of urea.
Described urea addition is the 20%-70% of the fine amount of relative first.
After the present invention adopts and earlier cellulose is alkalized, carry out mixed dissolution with urea liquid again, improved cellulosic solubility, and avoided cellulose alkalization under the precooling situation, the violent phenomenon of cellulose swollen in alkali lye, to the requirement of equipment, and production technology is simple, is fit to suitability for industrialized production when having reduced dissolving.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
With the degree of polymerization is that 450 cotton pulp is put into the dense alkali lye dipping alkalization for 150g/L of alkali 30 minutes, after alkalization temperature is 52 ℃, through squeezing and pulverizing, cellulose quality content is 15% in the alkali cellulose that makes, the alkali mass content is 8%, and after being cooled to room temperature, be transported to then in the reactor, add aqueous solution of urea in reactor, urea quality content is 10% in the aqueous solution of urea, the urea addition is 10% of the fine amount of relative first, after being cooled to-3 ℃, stir, to dissolving fully, in dissolving, carry out vacuum defoamation, make homogeneous, transparent spinning solution.
Embodiment 2
With the degree of polymerization is that 350 cotton pulp is put into the dense alkali lye dipping alkalization for 90g/L of alkali 40 minutes, after alkalization temperature is 45 ℃, through squeezing and pulverizing, the alkali cellulose cellulose quality content that makes is 18%, the alkali mass content is 8%, and after being cooled to room temperature, be transported in the reactor, add aqueous solution of urea in reactor, urea quality content is 15% in the aqueous solution of urea, and the urea addition is 20% of the fine content of relative first, after being cooled to 4 ℃, be stirred to fully dissolving, in dissolving, carry out vacuum defoamation, make homogeneous, transparent spinning solution.
Embodiment 3
With the degree of polymerization is that 390 cotton pulp is put into the dense alkali lye dipping alkalization for 180g/L of alkali 20 minutes, after alkalization temperature is 50 ℃, through squeezing and pulverizing, the alkali cellulose cellulose quality content that makes is 30%, the alkali mass content is 8%, and after being cooled to room temperature, be transported in the reactor that adds aqueous solution of urea in advance and mix, urea quality content is 10% in the aqueous solution of urea, the urea addition be relative first fibre contain 40%, be cooled to-3 ℃ after, be stirred to fully dissolving, in dissolving, carry out vacuum defoamation, make homogeneous, transparent spinning solution.
Embodiment 4
With the degree of polymerization is that 485 cotton pulp is put into the dense alkali lye dipping alkalization for 240g/L of alkali 10 minutes, after alkalization temperature is 54 ℃, the alkali cellulose cellulose quality content that makes after squeezing and pulverizing is 31%, the alkali mass content is 16%, and be cooled to room temperature, be transported in the reactor, in reactor, add aqueous solution of urea again, urea quality content is 15% in the aqueous solution of urea, the urea addition is 60% of the fine content of relative first, and after being cooled to 10 ℃, is stirred to dissolving fully, in dissolving, carry out vacuum defoamation, make homogeneous, transparent spinning solution.
Claims (6)
1, a kind of preparation technology of cellulose fibre spinning solution, it is characterized in that: adopt cellulose pulp through alkalization, squeezing and pulverizing, and after the cooling, mix with aqueous solution of urea, be cooled to-5 ℃～15 ℃ afterwards, alkali cellulose is dissolved in stirring, and carries out vacuum defoamation in dissolving, makes spinning solution.
2, the preparation technology of cellulose fibre spinning solution according to claim 1, it is characterized in that: used pulp is that the degree of polymerization is cotton pulp or the wood pulp of 300-500.
3, the preparation technology of cellulose fibre spinning solution according to claim 1, it is characterized in that: described alkalization temperature is 40-60 ℃, and alkali is dense to be 80-250g/L, and alkalization time is 5-50 minute.
4, the preparation technology of cellulose fibre spinning solution according to claim 1, it is characterized in that: the alkali cellulose cellulose quality content that makes is 10-40%, and the alkali mass content is 5-20%.
5, the preparation technology of cellulose fibre spinning solution according to claim 1, it is characterized in that: urea quality content is 5%-15% in the described aqueous solution of urea.
6, as the preparation technology of cellulose fibre spinning solution as described in each in the claim 1 to 5, it is characterized in that: described amount of urea is the 20%-70% of the fine amount of relative first.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810238473XA CN101435115A (en) | 2008-12-19 | 2008-12-19 | Preparation technique of cellulose fibre spinning solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810238473XA CN101435115A (en) | 2008-12-19 | 2008-12-19 | Preparation technique of cellulose fibre spinning solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101435115A true CN101435115A (en) | 2009-05-20 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200810238473XA Pending CN101435115A (en) | 2008-12-19 | 2008-12-19 | Preparation technique of cellulose fibre spinning solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101435115A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541801A (en) * | 2016-06-29 | 2018-01-05 | 吉林富博纤维研究院有限公司 | A kind of preparation method of cellulose spin dope |
| CN107779963A (en) * | 2016-08-25 | 2018-03-09 | 山东雅美科技有限公司 | The preparation of coloured flame-retardant anti-bacterial fibre cellulose fiber stoste |
-
2008
- 2008-12-19 CN CNA200810238473XA patent/CN101435115A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541801A (en) * | 2016-06-29 | 2018-01-05 | 吉林富博纤维研究院有限公司 | A kind of preparation method of cellulose spin dope |
| CN107779963A (en) * | 2016-08-25 | 2018-03-09 | 山东雅美科技有限公司 | The preparation of coloured flame-retardant anti-bacterial fibre cellulose fiber stoste |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090520 |