CN104233495B - A kind of salix monogolica regenerated cellulose and preparation method thereof - Google Patents

A kind of salix monogolica regenerated cellulose and preparation method thereof Download PDF

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CN104233495B
CN104233495B CN201410544050.6A CN201410544050A CN104233495B CN 104233495 B CN104233495 B CN 104233495B CN 201410544050 A CN201410544050 A CN 201410544050A CN 104233495 B CN104233495 B CN 104233495B
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salix monogolica
salix
monogolica
celulose fibre
spinning solution
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CN201410544050.6A
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Chinese (zh)
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CN104233495A (en
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钱景
赵兵
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钱景
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Abstract

The invention discloses a kind of salix monogolica regenerated cellulose and preparation method thereof, step is as follows: removed the peel by salix monogolica, pulverize, sieve, dry, cool preparation salix monogolica wood powder; Ethanol-sour mixed liquor is adopted to extract salix monogolica cellulose; By salix monogolica fiber obtained salix monogolica pulp after the PROCESS FOR TREATMENT such as boiling, bleaching; With salix monogolica pulp for raw material, through dipping, squeezing, pulverize, experienced, yellow, dissolving, deaeration and filtration step obtain spinning solution; By spinning solution through coagulating bath spinning, draw forming, then obtain salix monogolica regenerated cellulose through refining, oven dry.The present invention utilizes salix monogolica to produce regenerated celulose fibre, and raw material is sufficient, cheap, improves the utilization rate of salix monogolica resource simultaneously, by the huge economic benefit of generation and ecological benefits.

Description

A kind of salix monogolica regenerated cellulose and preparation method thereof
Technical field
The present invention relates to a kind of salix monogolica regenerated cellulose and preparation method thereof, belong to natural polymer and field of textiles.
Background technology
For a long time, cellulose is the key industry raw material of weaving, papermaking always, day by day be subject to people's attention with its recyclability, biodegradability and cost advantage, in medicine control, release tech, immobilization technology, biology sensor, membrane material, performance chemicals and additive etc., demonstrate good development prospect.Due to the minimizing in arable land and the day by day exhausted of the fossil resource such as oil, natural gas, the output of natural fabric, synthetic fiber will be subject to increasing restriction.And regenerated cellulose is as a kind of green, environmental protection, reproducible resource, obtain a unprecedented opportunity to develop.
Salix monogolica is the desert plant that a kind of only a few can grow in salt-soda soil.Its sprout is yellow, the linear or wire lanceolar in leaf, and branch is grown thickly and is not afraid of husky pressure, well developed root system, and rudiment power is strong, is desert-control tree, is mainly distributed in the ground such as the Inner Mongol, Hebei, Shanxi, Shaanxi, Gansu, Qinghai, Sichuan.Salix monogolica is one of the first-selection of " three Norths shelter-forest ", not only plays the effect of checking winds and fixing drifting sand, conserving water and soil, and is improving the function also in the ecosystem, the maintenance ecological balance etc. with uniqueness.
Salix monogolica is except small part is used for pulping and paper-making, fiberboard and composite plate, and the overwhelming majority is as yule logs burning or abandon, and causes the huge wasting of resources.The main chemical compositions of salix monogolica mainly contains cellulose, hemicellulose, lignin and ash content, and cellulosic content, at more than 60-70%, is natural reproducible biomass resource, and Appropriate application salix monogolica resource is by the huge economic benefit of generation and ecological benefits.At present, most research all concentrates on the cellulose how extracted in salix monogolica.Beijing Forestry University department of chemistry engineering Jiang builds and new waits people to have studied the impact (modern chemical industry, 2008,28 (2)) of steam blasting preliminary treatment on salix monogolica composition and fibre structure performance.The people such as Agricultural University of the Inner Mongol's material science and School of Art and Design Zhang Bin for raw material, have studied the technique (paper and papermaking, 2014,33 (3)) that supercritical ultrasonics technology prepares microfibril with salix monogolica cellulose.Main chemical compositions cellulose, the hemicellulose (Agricultural University of the Inner Mongol's journal, 2014,35 (1)) of Agricultural University of the Inner Mongol's material science and people utilized chemical reagent the to isolate salix monogolica material such as School of Art and Design Li Ya is refined.The people such as industry light industry textile industry institute of Qiqihar University Xu Feng utilize the cellulose (chemistry of forest product and industry, 2006,26 (2)) in hydrogen peroxide method separation salix monogolica and caragana microphylla mixed material.The people such as Zhengzhou University's chemical industry and the yellow star of energy institute adopt acid catalysis Ethanol Method to extract salix monogolica cellulose (Jiangsu's agriculture science, 2014,42 (3)).But there are no document by the salix monogolica cellulose that extracts for the preparation of salix monogolica regenerated cellulose.
At present, regenerated celulose fibre mainly with wood pulp, bamboo pulp, cotton pulp for raw material, be prepared from through viscose process or solvent method.But along with the minimizing of poor, the cultivated area of the forest reserves and bamboo wood need the restriction of the factors such as 3 year growth period, find the new raw material of exploitation and prepare regenerated celulose fibre and just become the task of top priority.
Summary of the invention
The present invention is directed to above-mentioned deficiency, a kind of preparation method of salix monogolica regenerated celulose fibre is provided.
The present invention is achieved by following technical proposals:
(1) salix monogolica wood powder is prepared: removed the peel by salix monogolica, pulverize, cross 50-100 mesh sieve, 80-100 DEG C of oven dry, cooling, puts into drier for subsequent use;
(2) salix monogolica cellulose is extracted: by the salix monogolica wood powder in step (1), add in autoclave, add absolute ethyl alcohol-sour mixed liquor, solid-to-liquid ratio 1:5-1:20, after being heated to 100-160 DEG C, stir 1-5h, cooling, filters, with absolute ethanol washing 2-5 time, repeatedly rinse well with deionized water again, dry;
(3) prepare salix monogolica pulp: the NaOH boiling adopting 5-15%wt, bath raio is 1:5-1:10, boiling temperature 200-250 DEG C, time 3-5h, then the hydrogen peroxide bleaching adopting 20-25%wt, bleaching temperature 80-100 DEG C, bleaching time 1-2h;
(4) prepare salix monogolica spinning solution: with salix monogolica pulp for raw material, through dipping, squeezing, pulverize, experienced, yellow, dissolving, deaeration and filtration step obtain spinning solution;
(5) prepare salix monogolica regenerated celulose fibre: by spinning solution through coagulating bath spinning, draw forming, then obtain salix monogolica regenerated celulose fibre through concise, oven dry.
Preferably, the acid in described step (2) is one or more in sulfuric acid, nitric acid, hydrochloric acid, acetic acid, and addition is 3-5%wt.
Preferably, the coagulation bath temperature in described step (5) is 40-60 DEG C, sulfur acid 100-130g/L, zinc sulfate 15-20g/L, sodium sulphate 320-360g/L in coagulating bath, drafting multiple 1.8-2.0.
Compared with prior art, the invention has the advantages that:
The present invention utilizes salix monogolica to produce regenerated celulose fibre, raw material is sufficient, cheap, improve the utilization rate of salix monogolica resource simultaneously, solve salix monogolica except small part is for except pulping and paper-making, fiberboard and composite plate, the overwhelming majority is as yule logs burning or abandon, and causes the problem of the huge wasting of resources, by the huge economic benefit of generation and ecological benefits.
Detailed description of the invention
Below in conjunction with detailed description of the invention, set forth the present invention further.
Embodiment 1:
(1) salix monogolica wood powder is prepared: removed the peel by salix monogolica, pulverize, cross 100 mesh sieves, 80 DEG C of oven dry, cooling, puts into drier for subsequent use;
(2) salix monogolica cellulose is extracted: by the salix monogolica wood powder in step (1), add in autoclave, add absolute ethyl alcohol-nitric acid mixed liquor, wherein nitric acid addition is 3%wt, solid-to-liquid ratio 1:10, after being heated to 120 DEG C, stir 3h, cooling, filter, with absolute ethanol washing 5 times, more repeatedly rinse well with deionized water, dry;
(3) prepare salix monogolica pulp: the NaOH boiling adopting 10%wt, bath raio is 1:10, boiling temperature 200 DEG C, time 3h, then the hydrogen peroxide bleaching adopting 20%wt, bleaching temperature 100 DEG C, bleaching time 2h;
(4) prepare salix monogolica spinning solution: with salix monogolica pulp for raw material, through dipping, squeezing, pulverize, experienced, yellow, dissolving, deaeration and filtration step obtain spinning solution;
(5) salix monogolica regenerated celulose fibre is prepared: by spinning solution through coagulating bath spinning, draw forming, then salix monogolica regenerated cellulose is obtained through concise, oven dry, wherein coagulation bath temperature is 60 DEG C, sulfur acid 100g/L, zinc sulfate 15g/L, sodium sulphate 320g/L in coagulating bath, drafting multiple 2.0.
The salix monogolica regenerated cellulose prepared according to embodiment 1 does strong 1.98cN/dtex, and wet strong 1.01cN/dtex, water free breaking elongation rate 21.3%, wet break elongation 12.81%, mechanical property is suitable with viscose.
Embodiment 2:
(1) salix monogolica wood powder is prepared: removed the peel by salix monogolica, pulverize, cross 80 mesh sieves, 90 DEG C of oven dry, cooling, puts into drier for subsequent use;
(2) salix monogolica cellulose is extracted: by the salix monogolica wood powder in step (1), add in autoclave, add absolute ethyl alcohol-sulfuric acid mixture liquid, wherein sulfuric acid addition is 4%wt, solid-to-liquid ratio 1:5, after being heated to 120 DEG C, stir 2h, cooling, filter, with absolute ethanol washing 3 times, more repeatedly rinse well with deionized water, dry;
(3) prepare salix monogolica pulp: the NaOH boiling adopting 5%wt, bath raio is 1:5, boiling temperature 250 DEG C, time 4h, then the hydrogen peroxide bleaching adopting 25%wt, bleaching temperature 80 DEG C, bleaching time 1h;
(4) prepare salix monogolica spinning solution: with salix monogolica pulp for raw material, through dipping, squeezing, pulverize, experienced, yellow, dissolving, deaeration and filtration step obtain spinning solution;
(5) salix monogolica regenerated celulose fibre is prepared: by spinning solution through coagulating bath spinning, draw forming, then salix monogolica regenerated cellulose is obtained through concise, oven dry, wherein coagulation bath temperature is 40 DEG C, sulfur acid 120g/L, zinc sulfate 20g/L, sodium sulphate 360g/L in coagulating bath, drafting multiple 1.8.
Embodiment 3:
(1) salix monogolica wood powder is prepared: removed the peel by salix monogolica, pulverize, cross 60 mesh sieves, 80 DEG C of oven dry, cooling, puts into drier for subsequent use;
(2) salix monogolica cellulose is extracted: by the salix monogolica wood powder in step (1), add in autoclave, add absolute ethyl alcohol-hydrochloric acid mixed solution, solid-to-liquid ratio 1:15, after being heated to 140 DEG C, stir 3h, cooling, filter, with absolute ethanol washing 2 times, more repeatedly rinse well with deionized water, dry;
(3) prepare salix monogolica pulp: the NaOH boiling adopting 15%wt, bath raio is 1:10, boiling temperature 220 DEG C, time 3h, then the hydrogen peroxide bleaching adopting 20%wt, bleaching temperature 80 DEG C, bleaching time 2h;
(4) prepare salix monogolica spinning solution: with salix monogolica pulp for raw material, through dipping, squeezing, pulverize, experienced, yellow, dissolving, deaeration and filtration step obtain spinning solution;
(5) salix monogolica regenerated celulose fibre is prepared: by spinning solution through coagulating bath spinning, draw forming, then salix monogolica regenerated cellulose is obtained through concise, oven dry, wherein coagulation bath temperature is 50 DEG C, sulfur acid 110g/L, zinc sulfate 15g/L, sodium sulphate 350g/L in coagulating bath, drafting multiple 1.9.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.

Claims (3)

1. a preparation method for salix monogolica regenerated celulose fibre, is characterized in that:
Step one, preparation salix monogolica wood powder: removed the peel by salix monogolica, pulverize, cross 50-100 mesh sieve, 80-100 DEG C of oven dry, cooling, puts into drier for subsequent use;
Step 2, extract salix monogolica cellulose: by the salix monogolica wood powder in step one, add in autoclave, add absolute ethyl alcohol-sour mixed liquor, solid-to-liquid ratio 1:5-1:20, be heated to 100-160 DEG C, stir 1-5h, cooling, filter, with absolute ethanol washing 2-5 time, more repeatedly rinse well with deionized water, dry;
Step 3, preparation salix monogolica pulp: employing mass fraction is the NaOH boiling of 5-15%, and bath raio is 1:5-1:10, boiling temperature 200-250 DEG C, time 3-5h, then adopt mass fraction to be the hydrogen peroxide bleaching of 20-25%, bleaching temperature 80-100 DEG C, bleaching time 1-2h;
Step 4, preparation salix monogolica spinning solution: with salix monogolica pulp for raw material, through dipping, squeezing, pulverize, experienced, yellow, dissolving, deaeration and filtration step obtain spinning solution;
Step 5, preparation salix monogolica regenerated celulose fibre: by spinning solution through coagulating bath spinning, draw forming, then obtains salix monogolica regenerated celulose fibre through concise, oven dry.
2. the preparation method of a kind of salix monogolica regenerated celulose fibre according to claim 1, is characterized in that, the acid described in step 2 is one or more in sulfuric acid, nitric acid, hydrochloric acid, acetic acid, and addition is 3-5%wt.
3. the preparation method of a kind of salix monogolica regenerated celulose fibre according to claim 1, it is characterized in that, coagulation bath temperature in step 5 is 40-60 DEG C, sulfur acid 100-130g/L, zinc sulfate 15-20g/L, sodium sulphate 320-360g/L in coagulating bath, drafting multiple 1.8-2.0.
CN201410544050.6A 2014-10-15 2014-10-15 A kind of salix monogolica regenerated cellulose and preparation method thereof CN104233495B (en)

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CN105887213B (en) * 2016-05-05 2018-01-12 安徽工程大学 A kind of preparation method and applications of purple willow chicken feather fibers
CN106368034A (en) * 2016-11-14 2017-02-01 哈尔滨工业大学 Method for extracting cellulose from traditional Chinese medicine dregs and application of cellulose
CN107556534A (en) * 2017-09-17 2018-01-09 钱景 A kind of salix monogolica konjaku composite and preparation method thereof
CN107446155A (en) * 2017-09-17 2017-12-08 钱景 A kind of nano ferriferrous oxide/three-dimensional porous the magnetic composite of salix monogolica/konjaku
CN107573712A (en) * 2017-09-17 2018-01-12 钱景 A kind of improved salix monogolica konjaku is composite porous and preparation method thereof
CN107573713A (en) * 2017-09-17 2018-01-12 钱景 A kind of salix monogolica konjaku beta cyclodextrin composite and preparation method thereof
CN107501633A (en) * 2017-09-17 2017-12-22 钱景 A kind of salix monogolica/konjaku/cyclodextrin composite and preparation method thereof
CN107540876A (en) * 2017-09-17 2018-01-05 钱景 A kind of magnetic nanometer composite material based on salix cellulose/konjaku
CN108299566B (en) * 2017-12-28 2020-09-29 潍坊友容实业有限公司 Process method for preparing regenerated cellulose by utilizing amorpha fruticosa planted in saline-alkali soil
CN108166089B (en) * 2017-12-28 2020-07-07 潍坊友容实业有限公司 Method for preparing regenerated cellulose by utilizing amorpha fruticosa planted in saline-alkali soil

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