CN106702514A - Regenerated cellulose fiber short filament - Google Patents
Regenerated cellulose fiber short filament Download PDFInfo
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- CN106702514A CN106702514A CN201510598448.2A CN201510598448A CN106702514A CN 106702514 A CN106702514 A CN 106702514A CN 201510598448 A CN201510598448 A CN 201510598448A CN 106702514 A CN106702514 A CN 106702514A
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Abstract
The invention discloses a regenerated cellulose fiber short filament. The regenerated cellulose fiber short filament is prepared via spinning of a spinning solution prepared via dissolving of cellulose amino acid methyl ester; dry breaking strength ranges from 2.1 to 2.4cN/dtex, wet breaking strength ranges from 1.1 to 1.3cN/dtex, dry elongation at break ranges from 10 to 15%, dry deviation coefficient of elongation ranges from 8 to 12%, and no residual sulfur is contained. The regenerated cellulose fiber short filament is high-strength low-elongation regenerated cellulose fiber; product performance is excellent; no residual sulfur is contained; and the regenerated cellulose fiber short filament can be applied in people's livelihood industries such as garment fabric, sewing thread, and tire cord.
Description
Technical field
The present invention is a kind of short silk of regenerated celulose fibre, and in particular in commercial process, by the synthesizing of cellulose carbamate, is dissolved and cellulose carbamate fibre short silk prepared by spinning, belongs to the production technical field of regenerated celulose fibre.
Background technology
In textile industry field, viscose rayon is to realize one of fiber of industrialized production at first, is developed rapidly due to its good performance and cheap cost.In traditional viscose glue production process, a number of pulp material and alkali lye effect generation alkali cellulose, then with CS2Cellulose xanthate is synthesized, viscose glue is prepared through the step such as dissolving, mixing, filtering, deaeration and maturation, then again through spinning, post processing, etc. operation viscose short-thread is obtained, be related to the synthesis of cellulose xanthate, dissolve and spining technology.Because the synthesis of cellulose xanthate needs to use CS2, easily environment is impacted, therefore, to reduce environmental protection pressure, the synthetic technology of the cellulose carbamate of alternative fiber element sodium sulfonate is increasingly becoming the emphasis and hot spot technology of the environmental protection research of Textile Industry industrial energy saving.
The synthetic route of known cellulose carbamate is included：（1）With cellulose pulp and urea as raw material, the synthesis method of fiber carbamate in atent solvent dimethylbenzene, such as：CN1687137（New technique for preparing cellulose carbate through urea embedding method, 2005.10.26）" synthesis of cellulose carbamate "（It is recorded in《Polymer material science and engineering》, the 4th phase of volume 21, in July, 2005）；（2）With cellulose pulp and urea as raw material, supercritical carbon dioxide fluid is carrier, esterification is completed under the assistance of cosolvent cellulose carbamate is obtained, such as：CN102702364A
（A kind of preparation method of cellulose carbamate, 2012.10.03）、CN102766216A（The preparation method of cellulose carbamate, 2012.11.07）And CN1775810（The method that cellulose carbamate is prepared using supercritical carbon dioxide, 2006.05.24）；（3）With cellulose and urea as raw material, cellulose carbamate is obtained after heated, reaction, drying, such as：CN104072622A（A kind of preparation of cellulose carbamate and its dissolution in low temperature spinning process, 2014.10.01）And CN104497151A（A kind of method of the urea-modified cellulose of no coupling product, 2015.04.08）, etc..In the industrial processes of viscose rayon, it is understood that, the process modification of single link can not weigh its industrialized practical value, just by taking the synthetic technology of above-mentioned cellulose carbamate as an example, existing open source literature only describes the synthetic route of cellulose carbamate, but in actual industrial production, from cellulose carbamate to during obtaining regenerated celulose fibre, also in the presence of such as：All too many levels such as dissolving, deaeration, spinning, drying, post-processing, therefore, even if preparing cellulose carbamate by said synthesis route, the energy-conserving and environment-protective for thoroughly solving the problems, such as industrialized production regenerated celulose fibre can not be also represented, it is also possible to situations below occur：One, the Testing index of the regenerated celulose fibre that the spinning solution that cellulose carbamate is prepared is obtained after spinning moulding is difficult to meet the requirement of downstream product；Two, the regenerated celulose fibre performance difference that cellulose carbamate is prepared is larger, and existing spinning head or draft apparatus are not suitable with spinning process, it is necessary to put into new equipment again, and production cost increases etc..
Patent document CN102691125A（A kind of method that regenerated celulose fibre is prepared by cellulose carbamate, 2012.09.26）Describe the process for obtaining regenerated celulose fibre after dissolving, freezing, defrosting, filtering, deaeration, spinning, solidification, washing, drying by cellulose carbamate, the dry fracture strength of the regenerated celulose fibre for preparing in the method is 1.44~2.86cN/dtex, wet breaking strength is 0.46~0.60 cN/dtex, dry elongation at break is 7~15%, it is seen from the above data that the preparation method faces problems with：One, the regenerated celulose fibre prepared by above-mentioned regenerated celulose fibre can not fully meet the requirement of the downstream product such as garment material, high intensity stocking yarn：Dry fracture strength >=2.1cN/dtex, wet breaking strength >=1.0cN/dtex, dry elongation at break ＞ 12%；Two, the regenerated celulose fibre that the method is prepared belongs to low strong flatness type, and intensity and elongation are relatively low, and spinning is more difficult, in actual spinning process, can not by the tow of existing spinning head extrusion molding, therefore, do not possess industrial utility value.
The content of the invention
It is an object of the invention to provide a kind of short silk of regenerated celulose fibre, the spinning solution spinning obtained using cellulose carbamate solvent is obtained the short silk of regenerated celulose fibre, the short silk of the regenerated celulose fibre meets dry fracture strength >=2.1cN/dtex, the characteristic of dry elongation at break≤12%, belong to high-tenacity low-elongation viscose rayon, with good product performance, the characteristic without residual sulphur, application field includes the people's livelihood articles for use such as garment material, high intensity stocking yarn, curtain.
The present invention is achieved through the following technical solutions：A kind of short silk of regenerated celulose fibre, is obtained by the spinning solution spinning obtained after the dissolving of cellulose amino acid methyl ester, meets following index：
Dry fracture strength 2.1~2.4cN/dtex, 1.0~1.3cN/dtex of wet breaking strength,
Dry elongation at break 12~18%, the dry extension at break coefficient of variation 8~12%,
Residual sulfur content is 0.
The present invention is dissolved using cellulose amino acid methyl ester and cellulose amino acid methyl ester solution is obtained（Spinning solution）, can alternative fiber element xanthate acid production spinning solution, it is to avoid CS in viscose glue production technology2Use, understand after testing, regenerated celulose fibre is obtained by the inventive method and belongs to high-tenacity low-elongation regenerated celulose fibre, with preferable wet strength and dry strength, it is suitable for various frivolous, the smooth dress materials of spinning, high intensity stocking yarn, sewing threads etc., because refusal uses CS in production technology2, therefore, residual sulfur content is zero in the viscose fiber filament that the present invention is prepared, and more highlights the environmental protection of textile product.
The whiteness of the short silk of regenerated celulose fibre is 70~75%, and oil applying rate is 0.15~0.3%, and its product has dyeability good, is difficult to form the characteristic of aberration.
Further, the dye uniformity of the short silk of the regenerated celulose fibre is more than 3.5 grades, with even dyeing, quick characteristic, it is adaptable to which its effect is especially protruded during garment material field.
Further, the regain of the short silk of the regenerated celulose fibre is 13~17%, the characteristic with low water suction, when being used for stocking yarn etc., with good comfort level.
Further, the limited oxygen index of the short silk of the regenerated celulose fibre is 19~20%, with certain anti-flammability, during for fields such as garment material, knitting fabrics, can strengthen the feature of product, improves the surcharge and purposes of product.
Cellulose carbamate is dissolved using NaOH and zinc oxide aqueous solution for solution is existing, so that the dissolution velocity for producing spinning solution is slow, dissolving high energy consumption, be not suitable for the problem of industrialization large-scale production, dissolving of the present invention to cellulose amino acid methyl ester is improved, in the present invention, the dissolving step of the cellulose amino acid methyl ester includes：
A：Cellulose carbamate is added in sodium hydrate aqueous solution, stirring mixing carries out first time mixed dissolution, obtains mixed once solution；
B：To aluminum oxide is added in mixed once solution, stirring mixing carries out second mixed dissolution, 1~2h is freezed at -5~5 DEG C, obtains secondary mixed solution；
C：Secondary mixed solution is thawed to room temperature, cellulose carbamate fibre spinning solution is obtained.
In described step A, the concentration of sodium hydrate aqueous solution is 6~10%, and sodium hydrate solid is with the mass ratio of cellulose carbamate（1~2）：1, in the quality of this naoh concentration scope and NaOH and cellulose carbamate is than scope, with preferable dissolubility.
In described step A, the temperature of first time mixed dissolution is -10~0 DEG C, and the time of first time mixed dissolution is 1~2h, the dissolving for being advantageously selected for cellulose carbamate of above-mentioned solution temperature and time.
In described step B, aluminum oxide is 1 with the mass ratio of cellulose amino acid formic acid esters：（4~8）, above-mentioned specific process parameters range ensures that dissolution velocity is most fast, it is also possible to operation temperature higher can be maintained in course of dissolution.
The present invention compared with prior art, with advantages below and beneficial effect：
（1）The present invention solves the problems, such as that the technique of existing production cellulose carbamate fibre cannot adapt to industrialization large-scale production, propose a production process for the completeness short silk of regenerated celulose fibre higher, the short silk of regenerated celulose fibre for preparing meets dry fracture strength >=2.1cN/dtex, the characteristic of dry elongation at break≤12%, belong to high-tenacity low-elongation regenerated celulose fibre, with good product performance, characteristic without residual sulphur, application field includes garment material, high intensity stocking yarn, sewing threads, the people's livelihood industry such as tire cord, spinning solution good spinnability, the short silk good product performance of regenerated celulose fibre obtained through spinning, it is especially suitable for industrialization large-scale production, take into account production cost, production efficiency and product quality.
（2）The present invention is solved and existing dissolves cellulose carbamate using NaOH and zinc oxide aqueous solution, so that the dissolution velocity for producing spinning solution is slow, dissolving high energy consumption, be not suitable for the problem of industrialization large-scale production, by specific processing step and technological parameter, completeness cellulose carbamate fibre spinning solution production process higher is formed, the dissolving operation temperature of cellulose carbamate is higher（- 5~5 DEG C）, the technique can improve the dissolution velocity of cellulose carbamate, and reducing energy consumption, improve production efficiency, suitable to industrialize large-scale production.
（3）The short silk of regenerated celulose fibre of the present invention has preferable application value, and from the point of view of its index parameter, dye uniformity possesses even dyeing, quick characteristic more than 3.5 grades, it is adaptable to which its effect is especially protruded during garment material field；Regain meets 13~17%, and the characteristic with high water absorption can improve the comfort level of fabric；Limited oxygen index meets 19~20%, possesses certain anti-flammability, during for fields such as garment material, household articles, can strengthen the feature of product, improves value of the product and purposes.
（4）In production technology of the invention, CS2 is not used, therefore, from the point of view of the index parameter of the short silk of regenerated celulose fibre, residual sulfur content is zero, more highlights the environmental protection of textile product, is suitably widely popularized and uses.
Specific embodiment
The present invention is described in further detail with reference to embodiment, but embodiments of the present invention not limited to this.
Embodiment 1：
The present embodiment proposes a kind of short silk of regenerated celulose fibre, and the short silk of the regenerated celulose fibre is obtained by the spinning solution spinning obtained after the dissolving of cellulose amino acid methyl ester, meets following index：
Dry fracture strength 2.1cN/dtex, wet breaking strength 1.0cN/dtex,
Dry elongation at break 12%, the dry extension at break coefficient of variation 8%,
Residual sulfur content is 0.
Embodiment 2：
The short silk of regenerated celulose fibre that the present embodiment is related to is obtained by the spinning solution spinning obtained after the dissolving of cellulose amino acid methyl ester, meets following index：
Dry fracture strength 2.4cN/dtex, wet breaking strength 1.3cN/dtex,
Dry elongation at break 18%, the dry extension at break coefficient of variation 12%,
Residual sulfur content is 0.
Embodiment 3：
The present embodiment is on the basis of embodiment 1, and other index parameters to the short silk of regenerated celulose fibre are optimized, as follows：The whiteness of the short silk of regenerated celulose fibre is 70%, and oil applying rate is 0.15%.
Embodiment 4：
The present embodiment is on the basis of embodiment 2, and other index parameters to the short silk of regenerated celulose fibre are optimized, as follows：The whiteness of the short silk of regenerated celulose fibre is 75%, and oil applying rate is 0.3%.
Embodiment 5：
Dye uniformity of the present embodiment to the short silk of regenerated celulose fibre on the basis of embodiment 1 is defined, and in the present embodiment, the dye uniformity of the short silk of regenerated celulose fibre is 3.5 grades.
Embodiment 6：
Dye uniformity of the present embodiment to the short silk of regenerated celulose fibre on the basis of embodiment 2 is defined, and in the present embodiment, the dye uniformity of the short silk of regenerated celulose fibre is 5 grades.
Embodiment 7：
Regain of the present embodiment to the short silk of regenerated celulose fibre on the basis of embodiment 1 is defined, and in the present embodiment, the regain of the short silk of regenerated celulose fibre is 13%.
Embodiment 8：
Regain of the present embodiment to the short silk of regenerated celulose fibre on the basis of embodiment 2 is defined, and in the present embodiment, the regain of the short silk of regenerated celulose fibre is 17%.
Embodiment 9：
Limited oxygen index of the present embodiment to the short silk of regenerated celulose fibre on the basis of embodiment 1 is defined, and in the present embodiment, the limited oxygen index of the short silk of regenerated celulose fibre is 19%.
Embodiment 10：
Limited oxygen index of the present embodiment to the short silk of regenerated celulose fibre on the basis of embodiment 2 is defined, and in the present embodiment, the limited oxygen index of the short silk of regenerated celulose fibre is 20%.
Embodiment 11：
The present embodiment is on the basis of embodiment 1, it is proposed that the dissolving step of cellulose amino acid methyl ester includes in the short silk production process of regenerated celulose fibre：
A：Cellulose carbamate is added in sodium hydrate aqueous solution, stirring mixing carries out first time mixed dissolution, obtains mixed once solution；
B：To aluminum oxide is added in mixed once solution, stirring mixing carries out second mixed dissolution, 1h is freezed at -5 DEG C, obtains secondary mixed solution；
C：Secondary mixed solution is thawed to room temperature, cellulose carbamate fibre spinning solution is obtained.
Embodiment 12：
The present embodiment is on the basis of embodiment 2, it is proposed that the dissolving step of cellulose amino acid methyl ester includes in the short silk production process of regenerated celulose fibre：
A：Cellulose carbamate is added in sodium hydrate aqueous solution, stirring mixing carries out first time mixed dissolution, obtains mixed once solution；
B：To aluminum oxide is added in mixed once solution, stirring mixing carries out second mixed dissolution, 2h is freezed at 5 DEG C, obtains secondary mixed solution；
C：Secondary mixed solution is thawed to room temperature, cellulose carbamate fibre spinning solution is obtained.
Embodiment 13：
The present embodiment is with the difference of embodiment 11：The step of the present embodiment is related in A, the concentration of sodium hydrate aqueous solution is 6%, and sodium hydrate solid is 1 with the mass ratio of cellulose carbamate：1.
Embodiment 14：
The present embodiment is with the difference of embodiment 12：The step of the present embodiment is related in A, the concentration of sodium hydrate aqueous solution is 10%, and sodium hydrate solid is 2 with the mass ratio of cellulose carbamate：1.
Embodiment 15：
The present embodiment is with the difference of embodiment 11：The step of the present embodiment is related in A, the temperature of first time mixed dissolution is -10 DEG C, and the time of first time mixed dissolution is 1h.
Embodiment 16：
The present embodiment is with the difference of embodiment 12：The step of the present embodiment is related in A, the temperature of first time mixed dissolution is 0 DEG C, and the time of first time mixed dissolution is 2h.
Embodiment 17：
The present embodiment is with the difference of embodiment 11：The step of the present embodiment is related in B, aluminum oxide is 1 with the mass ratio of cellulose amino acid formic acid esters：4.
Embodiment 18：
The present embodiment is with the difference of embodiment 12：The step of the present embodiment is related in B, aluminum oxide is 1 with the mass ratio of cellulose amino acid formic acid esters：8.
Embodiment 19：
The short silk of regenerated celulose fibre that the present embodiment is related to meets：
Dry fracture strength 2.4cN/dtex, wet breaking strength 1.2cN/dtex,
Dry elongation at break 15.8%, the dry extension at break coefficient of variation 11.7%,
Residual sulfur content is 0, and whiteness is 75%, and oil applying rate is 0.22%,
Dye uniformity is 3.5 grades, and regain is 16%,
Limited oxygen index is 19.2%.
The preparation technology of the above-mentioned short silk of regenerated celulose fibre is as follows：
A：Cellulose carbamate is added in the sodium hydrate aqueous solution that concentration is 8%, stirring mixing carries out first time mixed dissolution, solution temperature is -5 DEG C, after dissolving 1h, obtains mixed once solution, wherein, sodium hydrate solid and the mass ratio of cellulose carbamate are 1.5：1；
B：To aluminum oxide is added in mixed once solution, stirring mixing carries out second mixed dissolution, 2h is freezed at 2.5 DEG C, obtains secondary mixed solution, wherein, aluminum oxide is 1 with the mass ratio of cellulose amino acid formic acid esters：5；
C：Secondary mixed solution is thawed to room temperature, cellulose carbamate fibre spinning solution is obtained；
D：The spinning of cellulose carbamate fibre spinning solution is obtained the short silk of regenerated celulose fibre.
Embodiment 20：
The short silk of regenerated celulose fibre that the present embodiment is related to meets：
Dry fracture strength 2.1cN/dtex, wet breaking strength 1.23cN/dtex,
Dry elongation at break 16%, the dry extension at break coefficient of variation 10.8%,
Residual sulfur content is 0, and whiteness is 72%, and oil applying rate is 0.2%,
Dye uniformity is 4 grades, and regain is 14%,
Limited oxygen index is 19%.
The preparation technology of the above-mentioned short silk of regenerated celulose fibre is as follows：
A：Cellulose carbamate is added in the sodium hydrate aqueous solution that concentration is 9%, stirring mixing carries out first time mixed dissolution, solution temperature is -6 DEG C, after dissolving 1.5h, obtains mixed once solution, wherein, sodium hydrate solid and the mass ratio of cellulose carbamate are 1.8：1；
B：To aluminum oxide is added in mixed once solution, stirring mixing carries out second mixed dissolution, 2h is freezed at 0 DEG C, obtains secondary mixed solution, wherein, aluminum oxide is 1 with the mass ratio of cellulose amino acid formic acid esters：6；
C：Secondary mixed solution is thawed to room temperature, cellulose carbamate fibre spinning solution is obtained；
D：The spinning of cellulose carbamate fibre spinning solution is obtained the short silk of regenerated celulose fibre.
Embodiment 21：
The short silk of regenerated celulose fibre that the present embodiment is related to meets：
Dry fracture strength 2.2cN/dtex, wet breaking strength 1.25cN/dtex,
Dry elongation at break 17.4%, the dry extension at break coefficient of variation 11%,
Residual sulfur content is 0, and whiteness is 73%, and oil applying rate is 0.17%,
Dye uniformity is 4 grades, and regain is 15%,
Limited oxygen index is 19.1%.
The preparation technology of the above-mentioned short silk of regenerated celulose fibre is as follows：
A：Cellulose carbamate is added in the sodium hydrate aqueous solution that concentration is 10%, stirring mixing carries out first time mixed dissolution, solution temperature is -8 DEG C, after dissolving 1.2h, obtains mixed once solution, wherein, sodium hydrate solid and the mass ratio of cellulose carbamate are 1：1；
B：To aluminum oxide is added in mixed once solution, stirring mixing carries out second mixed dissolution, 1h is freezed at -2.5 DEG C, obtains secondary mixed solution, wherein, aluminum oxide is 1 with the mass ratio of cellulose amino acid formic acid esters：7；
C：Secondary mixed solution is thawed to room temperature, cellulose carbamate fibre spinning solution is obtained；
D：The spinning of cellulose carbamate fibre spinning solution is obtained the short silk of regenerated celulose fibre.
Embodiment 22：
The short silk of regenerated celulose fibre that the present embodiment is related to meets：
Dry fracture strength 2.25cN/dtex, wet breaking strength 1.18cN/dtex,
Dry elongation at break 16.6%, the dry extension at break coefficient of variation 10.2%,
Residual sulfur content is 0, and whiteness is 74%, and oil applying rate is 0.16%,
Dye uniformity is 4.5 grades, and regain is 14.7%,
Limited oxygen index is 19%.
The preparation technology of the above-mentioned short silk of regenerated celulose fibre is as follows：
A：Cellulose carbamate is added in the sodium hydrate aqueous solution that concentration is 8%, stirring mixing carries out first time mixed dissolution, solution temperature is -5 DEG C, after dissolving 1h, obtains mixed once solution, wherein, sodium hydrate solid and the mass ratio of cellulose carbamate are 2：1；
B：To aluminum oxide is added in mixed once solution, stirring mixing carries out second mixed dissolution, 2h is freezed at -4 DEG C, obtains secondary mixed solution, wherein, aluminum oxide is 1 with the mass ratio of cellulose amino acid formic acid esters：5；
C：Secondary mixed solution is thawed to room temperature, cellulose carbamate fibre spinning solution is obtained；
D：The spinning of cellulose carbamate fibre spinning solution is obtained the short silk of regenerated celulose fibre.
The index parameter of the short silk of regenerated celulose fibre in above-described embodiment 1~22 is counted, as shown in table 1, table 2.
Table 1
Table 2
The average value of each index parameter of Example 1~22 is compared with the index parameter of regenerated celulose fibre in patent document CN102691125A respectively, as shown in table 3.
Table 3
Compared from above-mentioned data, the short silk of regenerated celulose fibre of the present invention belongs to high-tenacity low-elongation viscose rayon, application field includes the people's livelihood industry such as garment material, household goods.From the point of view of the data target of documents CN102691125A, regenerated celulose fibre disclosed in documents belongs to low strong flatness type regenerated celulose fibre（Intensity inside most of embodiment is less than 1.7）, application field includes socks, clothes dress material etc., has the shortcomings that intensity is relatively low, elasticity is poor, separately, because the performance of the product is larger with differing for viscose rayon, industrialized production is also difficult to use at present, and market popularization value is low.
The above, is only presently preferred embodiments of the present invention, and any formal limitation is not done to the present invention, and every any simple modification, equivalent variations made to above example according to technical spirit of the invention are each fallen within protection scope of the present invention.
Claims (9)
1. the short silk of a kind of regenerated celulose fibre, it is characterised in that：It is obtained by the spinning solution spinning obtained after the dissolving of cellulose amino acid methyl ester, meets following index：
Dry fracture strength 2.1~2.4cN/dtex, 1.0~1.3cN/dtex of wet breaking strength,
Dry elongation at break 12~18%, the dry extension at break coefficient of variation 8~12%,
Residual sulfur content is 0.
2. the short silk of a kind of regenerated celulose fibre according to claim 1, it is characterised in that：The whiteness of the short silk of regenerated celulose fibre is 70~75%, and oil applying rate is 0.15~0.3%.
3. the short silk of a kind of regenerated celulose fibre according to claim 1, it is characterised in that：The dye uniformity of the short silk of regenerated celulose fibre is more than 3.5 grades.
4. the short silk of a kind of regenerated celulose fibre according to claim 1, it is characterised in that：The regain of the short silk of regenerated celulose fibre is 13~17%.
5. the short silk of a kind of regenerated celulose fibre according to claim 1, it is characterised in that：The limited oxygen index of the short silk of regenerated celulose fibre is 19~20%.
6. the short silk of a kind of regenerated celulose fibre according to claim 1, it is characterised in that：The dissolving step of the cellulose amino acid methyl ester includes：
A：Cellulose carbamate is added in sodium hydrate aqueous solution, stirring mixing carries out first time mixed dissolution, obtains mixed once solution；
B：To aluminum oxide is added in mixed once solution, stirring mixing carries out second mixed dissolution, 1~2h is freezed at -5~5 DEG C, obtains secondary mixed solution；
C：Secondary mixed solution is thawed to room temperature, cellulose carbamate fibre spinning solution is obtained.
7. the short silk of a kind of regenerated celulose fibre according to claim 6, it is characterised in that：In described step A, the concentration of sodium hydrate aqueous solution is 6~10%, and sodium hydrate solid is with the mass ratio of cellulose carbamate（1~2）：1.
8. the short silk of a kind of regenerated celulose fibre according to claim 6, it is characterised in that：In described step A, the temperature of first time mixed dissolution is -10~0 DEG C, and the time of first time mixed dissolution is 1~2h.
9. the short silk of a kind of regenerated celulose fibre according to claim 6, it is characterised in that：In described step B, aluminum oxide is 1~2% with the mass ratio of cellulose amino acid formic acid esters.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101104957A (en) * | 2007-08-20 | 2008-01-16 | 中国科学院新疆理化技术研究所 | Process for preparing cellulose carbamate fibre |
| CN102691125A (en) * | 2012-06-19 | 2012-09-26 | 武汉大学 | Method for preparing regenerated cellulose fibers with cellulose carbamate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101104957A (en) * | 2007-08-20 | 2008-01-16 | 中国科学院新疆理化技术研究所 | Process for preparing cellulose carbamate fibre |
| CN102691125A (en) * | 2012-06-19 | 2012-09-26 | 武汉大学 | Method for preparing regenerated cellulose fibers with cellulose carbamate |
Non-Patent Citations (1)
| Title |
|---|
| 哈丽丹•买买提等: "尿素嵌入法生产纤维素氨基甲酸酯新工艺"", 《纤维素科学与技术》 * |
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