CN102635008B - Technique for producing dissolving pulp from whole cotton stalks - Google Patents
Technique for producing dissolving pulp from whole cotton stalks Download PDFInfo
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- CN102635008B CN102635008B CN201210138985.5A CN201210138985A CN102635008B CN 102635008 B CN102635008 B CN 102635008B CN 201210138985 A CN201210138985 A CN 201210138985A CN 102635008 B CN102635008 B CN 102635008B
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Abstract
The invention relates to the technical filed of a dissolving pulp, in particular to a technique for producing a dissolving pulp from whole cotton stalks. The technique comprises the steps of adding a hydrolysis accessory ingredient a into cotton stalks; performing pre-hydrolysis at a certain temperature for a certain time; carrying out KP/AQ cooking for the hydrolyzed pulp; performing OHP bleaching on the cooked pulp in three stages; and adding a hydrolysis accessory ingredient b into the bleached pulp for post-hydrolysis to obtain the dissolving pulp. According to the technique for producing the dissolving pulp from whole cotton stalks, hemi-cellulose is greatly dissolved out from the cotton stalks with the help of the pre-hydrolysis of the added accessory ingredient firstly; finally the content of the hemi-cellulose in the cotton stalks is further reduced by the post-hydrolysis of the added accessory ingredient; the processes of KP/AQ cooking and OHP bleaching are combined to prepare the cotton stalk dissolving pulp which is high in alpha-cellulose content, low in pentosan content, low in hemi-cellulose content and high in reactivity; and the adopted chemical products are clean and environment-friendly by utilization of the technique provided by the invention for processing whole cotton stalks.
Description
technical field
The present invention relates to dissolving pulp technical field, particularly a kind of technique of utilizing whole-cotton stalk to produce dissolving pulp.
background technology
Dissolving pulp is mainly as the raw material of artificial cotton, artificial silk, polynosic, the powerful cord fabric thread of tire, acetate fiber, enteric solubility tablet sugar-coat, medical artificial kidney, cigarette filter, cinefilm, carboxymethyl cellulose, nitrocellulose and bulletproof jacket made of paper, purposes is very wide, has now become modern light, spins, one of the important source material of the industry such as medicine, chemical industry, military project.
The main raw material that domestic dissolving pulp is produced is cotton linter, but due to the increase of viscose glue output in recent years, the demand of raw material is increased, and cotton linter can not meet the demand of chemical fibre industry to it, and exploitation new raw material is imperative.The domestic research and discovery practice of having carried out this respect, mainly adopting bamboo chip and wood chip is raw material, through prehydrolysis-alkaline cooking-bleaching, makes dissolving pulp.
Cotton stalk is as agricultural wastes, within 2004, the cotton stalk output of China is approximately more than 1,900 ten thousand tons, concerning whole-cotton stalk, average fiber length is about 1mm, width approximately 22 μ m, content of cellulose is about 38%, and wherein alpha-cellulose content is about 25%, if can utilize cotton stalk to prepare dissolving pulp, by of great advantage to the exploitation of dissolving pulp raw material.
summary of the invention
In order to solve, to take cotton linter and prepare as raw material the problem that dissolving pulp can not meet demand above, the invention provides a kind of technique of utilizing whole-cotton stalk to produce dissolving pulp.
The present invention is achieved in the following ways:
Utilize whole-cotton stalk to produce a technique for dissolving pulp, comprise the following steps:
(1) in cotton stalk, add hydrolysis auxiliary agent a, a period of time of prehydrolysis at a certain temperature;
(2) slurry after hydrolysis carries out KP/AQ boiling;
(3) slurry after boiling carries out OHP tri-stage bleaching;
(4) slurry after bleaching adds hydrolysis auxiliary agent b to carry out rear hydrolysis, obtains.
Described hydrolysis auxiliary agent a is that boric acid and aliphatic alcohol polyoxyvinethene phosphate are mixed to get according to mass ratio 1:1.
Described hydrolysis auxiliary agent b is aliphatic amine polyoxyethylene ether.
Pre-hydrolysis technique condition is: liquor ratio 1:4～8, and hydrolysis auxiliary agent a consumption is 0.1～0.5% of cotton stalk quality, temperature is 150～170 ℃, temperature retention time 90～180 minutes.
KP/AQ cooking schedule is: alkali charge is 15～25%, liquor ratio 1:3～6, and sulphidity is that 2.5～10%, AQ consumption is the 0.01-0.05% of oven dry stock quality, Tmax=160 ℃ ± 5 ℃, 30～90 minutes heating-up times, temperature retention time 90～180 minutes.
It is 0.4～0.6Mpa that oxygen that in OHP tri-stage bleaching, O floats is pressed, starch dense 10%, MgSO
4consumption is 0.5% of oven dry stock quality, and NaOH consumption is 1～3% of oven dry stock quality, 95～110 ℃ of temperature, insulation 60min.
In OHP tri-stage bleaching, H bleaching conditions is: T=45 ± 5 ℃, and in 60～120 minutes reaction time, Lime Quality concentration is 5～10%, pH=9～10, effective chlorine consumption is 1.0～3.0% of oven dry stock quality.
The MgSO that in OHP tri-stage bleaching, P floats
4consumption is 0.5% of oven dry stock quality, and NaOH consumption is 0.4% of oven dry stock quality, H
2o
2consumption is 3% of oven dry stock quality, starch dense 10%, 80～95 ℃ of temperature, reaction time 60～180min.
Rear hydrolysis process condition is: liquor ratio 1:6～10, hydrolysis auxiliary agent b consumption is 0.05～0.30% of oven dry stock quality, 100～140 ℃ of temperature, temperature retention time 90～180 minutes.
In KP/AQ boiling, AQ refers to anthraquinone.
First by means of the prehydrolysis of adding auxiliary agent, significantly deviate from the hemicellulose in cotton stalk, then adopt the KP/AQ boiling of low state of cure, the lignin of trying one's best, protection cellulose, reduce the discharge of boiling foul smell (foul smell is mainly the methyl mercaptan that vulcanized sodium and lignin reaction produce simultaneously, the lower-molecular substances such as dimethyl sulphide), boiling disposed slurry carries out the viscosity that OHP bleaching is further deviate from lignin and regulated dissolving pulp, finally, the rear hydrolysis of adding auxiliary agent to floating rear slurry further reduces the hemicellulose in dissolving pulp, the reactivity worth of content of ashes and raising dissolving pulp (CS while being mainly the production of raising later stage viscose glue
2diffusion rate).Adopt after this PROCESS FOR TREATMENT, the alpha-cellulose content in dissolving pulp improves, poly-pentose content reduces, hemicellulose level reduces, reactivity worth improves.
Beneficial effect of the present invention:
(1) first by means of the prehydrolysis of the adding auxiliary agent hemicellulose in the cotton stalk of stripping significantly, finally take the rear hydrolysis of adding auxiliary agent that the hemicellulose in cotton stalk is further reduced, in conjunction with KP/AQ boiling and OHP bleaching, prepared the cotton stalk dissolving pulp of high alpha-cellulose content, oligomeric pentose content, low hemicellulose level and high response energy again;
(2) adopt PROCESS FOR TREATMENT whole-cotton stalk of the present invention, chemicals clean environment firendly used.
The specific embodiment
For a better understanding of the present invention, below in conjunction with instantiation, further illustrate.
The hydrolysis auxiliary agent a using in following embodiment is mixed to get according to mass ratio 1:1 for boric acid and aliphatic alcohol polyoxyvinethene phosphate, and hydrolysis auxiliary agent b is aliphatic amine polyoxyethylene ether.
Embodiment 1: the rear hydrolysis process that adds prehydrolysis-KP/AQ-OHP-interpolation auxiliary agent of auxiliary agent is processed cotton stalk raw material
(1) get the whole-cotton stalk of the 20-40mm Chang Mount east product of 500g, its poly-pentose content is 18.3%, the pre-hydrolysis technique condition of controlling interpolation hydrolysis auxiliary agent a is: liquor ratio 1:4, hydrolysis auxiliary agent a dosage is 0.2% of cotton bar quality, 150 ℃ of maximum temperatures, temperature retention time 90 minutes, after hydrolysis, poly-pentose content is 7.2%, hydrolysis yield 84%;
(2) slurry after hydrolysis carries out KP/AQ boiling;
(3) slurry after boiling carries out OHP tri-stage bleaching;
(4) the rear hydrolysis process condition of interpolation auxiliary agent is: liquor ratio 1:6, hydrolysis auxiliary agent b consumption is 0.05% of oven dry stock quality, 100 ℃ of maximum temperatures, temperature retention time 180 minutes.
The alpha-cellulose content that obtains whole-cotton stalk pulp is 91%, and poly-pentose is 3.45%, viscosity 380ml/g, and whiteness 80%ISO, reactivity worth is 160 seconds.Every detection index of dissolving pulp is better, can be used to produce the fiber product of low whiteness.
In above-described embodiment, KP/AQ boiling and OHP tri-stage bleaching process conditions can realize technique effect of the present invention for the habitual process conditions of those skilled in the art, there is no special requirement, as:
KP/AQ cooking schedule: alkali charge is 15% of oven dry stock quality, liquor ratio 1:3, sulphidity is that 10%, AQ consumption is 0.05%, Tmax=160 ℃ ± 5 ℃, 30 minutes heating-up times, temperature retention time 90 minutes;
OHP tri-stage bleaching process conditions: oxygen that O floats is pressed as 0.4Mpa, starch dense 10%, MgSO
4consumption is 0.5% of oven dry stock quality, and NaOH consumption is 1% of oven dry stock quality, 95 ℃ of temperature, insulation 60min.; H bleaching conditions is: T=45 ± 5 ℃, 60 minutes reaction time, starch dense 10%, pH=9～10, effective chlorine consumption is 1.0% of oven dry stock quality; The MgSO that P floats
4for 0.5% of oven dry stock quality, NaOH is 0.4% of oven dry stock quality, H
2o
2for 3% of oven dry stock quality, starch dense 10%, 80 ℃ of temperature, reaction time 60min;
Embodiment 2: the rear hydrolysis process that adds prehydrolysis-KP/AQ-OHP-interpolation auxiliary agent of auxiliary agent is processed cotton stalk raw material
(1) get the whole-cotton stalk of the long Xinjiang of the 20-40mm product of 500g, its poly-pentose content is 20.1%, the pre-hydrolysis technique condition of controlling interpolation auxiliary agent is: liquor ratio 1:8, hydrolysis auxiliary agent a dosage is 0.2% of cotton bar quality, 170 ℃ of maximum temperatures, temperature retention time 180 minutes, after hydrolysis, poly-pentose content is 7.8%, hydrolysis yield 82%;
(2) slurry after hydrolysis carries out KP/AQ boiling;
(3) slurry after boiling carries out OHP tri-stage bleaching;
(4) the rear hydrolysis process condition of interpolation auxiliary agent is: liquor ratio 1:10, hydrolysis auxiliary agent b consumption is 0.30% of oven dry stock quality, 140 ℃ of maximum temperatures, temperature retention time 90 minutes.
The alpha-cellulose content that obtains whole-cotton stalk pulp is 90%, and poly-pentose is 3.6%, viscosity 370ml/g, and whiteness 79%ISO, reactivity worth is 175 seconds.
In above-described embodiment, KP/AQ boiling and OHP tri-stage bleaching process conditions can realize technique effect of the present invention for the habitual process conditions of those skilled in the art, there is no special requirement, as:
KP/AQ cooking schedule is: alkali charge is 25% of oven dry stock quality, liquor ratio 1:6, and sulphidity is that 2.5%, AQ consumption is 0.01%, Tmax=160 ℃ ± 5 ℃, 90 minutes heating-up times, temperature retention time 180 minutes;
OHP tri-stage bleaching process conditions: oxygen that O floats is pressed as 0.6Mpa, starch dense 10%, MgSO
4consumption is 0.5% of oven dry stock quality, and NaOH consumption is 3% of oven dry stock quality, 110 ℃ of temperature, insulation 60min.; H bleaching conditions is: T=45 ± 5 ℃, 120 minutes reaction time, starch dense 5%, C=10%, pH=9～10, effective chlorine consumption is 3.0% of oven dry stock quality; The MgSO that P floats
4for 0.5% of oven dry stock quality, NaOH is 0.4% of oven dry stock quality, H
2o
2for 3% of oven dry stock quality, starch dense 10%, 95 ℃ of temperature, reaction time 180min;
Embodiment 3:
Hydrolysis auxiliary agent a in embodiment 2 is changed to sulfuric acid by boric acid and aliphatic alcohol polyoxyvinethene phosphate, uses the cotton bar of equal in quality specification, after hydrolysis, poly-pentose content is 8.6%, hydrolysis yield 81%,
Step (2), (3), (4) are in full accord with embodiment 2, and the alpha-cellulose content of last gained whole-cotton stalk pulp is 88%, and poly-pentose is 4.8%, viscosity 350ml/g, and whiteness 78%ISO, reactivity worth is 220 seconds.
Claims (6)
1. utilize whole-cotton stalk to produce a technique for dissolving pulp, it is characterized in that comprising the following steps:
(1) in cotton bar, add hydrolysis auxiliary agent a, the a period of time of prehydrolysis at a certain temperature, pre-hydrolysis technique condition is: liquor ratio 1:4～8, and hydrolysis auxiliary agent a consumption is 0.1～0.5% of cotton bar quality, temperature is 150～170 ℃, temperature retention time 90～180 minutes;
(2) slurry after hydrolysis carries out KP/AQ boiling;
(3) slurry after boiling carries out OHP tri-stage bleaching;
(4) slurry after bleaching adds hydrolysis auxiliary agent b to carry out rear hydrolysis, and rear hydrolysis process condition is: liquor ratio 1:6～10, and hydrolysis auxiliary agent b consumption is 0.05～0.30% of oven dry stock quality, 100～140 ℃ of temperature, temperature retention time 90～180 minutes, obtains;
Described hydrolysis auxiliary agent a is that boric acid and aliphatic alcohol polyoxyvinethene phosphate are mixed to get according to mass ratio 1:1;
Described hydrolysis auxiliary agent b is aliphatic amine polyoxyethylene ether.
2. technique according to claim 1, it is characterized in that KP/AQ cooking schedule is: alkali charge is 15～25%, liquor ratio 1:3～6, sulphidity is 2.5～10%, AQ consumption is the 0.01-0.05% of oven dry stock quality, Tmax=160 ℃ ± 5 ℃, 30～90 minutes heating-up times, temperature retention time 90～180 minutes.
3. technique according to claim 1, is characterized in that it is 0.4～0.6MPa that oxygen that in OHP tri-stage bleaching, O floats is pressed, starch dense 10%, MgSO
4consumption is 0.5% of oven dry stock quality, and NaOH consumption is 1～3% of oven dry stock quality, 95～110 ℃ of temperature, insulation 60min.
4. technique according to claim 1, is characterized in that in OHP tri-stage bleaching, H bleaching conditions is: T=45 ± 5 ℃, and in 60～120 minutes reaction time, starching dense is 5～10%, pH=9～10, effective chlorine consumption is 1.0～3.0% of oven dry stock quality.
5. technique according to claim 1, is characterized in that the MgSO that in OHP tri-stage bleaching, P floats
4consumption is 0.5% of oven dry stock quality, and NaOH consumption is 0.4% of oven dry stock quality, H
2o
2consumption is 3% of oven dry stock quality, starch dense 10%, 80～95 ℃ of temperature, reaction time 60～180min.
6. technique according to claim 1, is characterized in that cotton bar is ground into 20-40mm long.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210138985.5A CN102635008B (en) | 2012-05-08 | 2012-05-08 | Technique for producing dissolving pulp from whole cotton stalks |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210138985.5A CN102635008B (en) | 2012-05-08 | 2012-05-08 | Technique for producing dissolving pulp from whole cotton stalks |
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| Publication Number | Publication Date |
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| CN102635008A CN102635008A (en) | 2012-08-15 |
| CN102635008B true CN102635008B (en) | 2014-02-26 |
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| CN201210138985.5A Expired - Fee Related CN102635008B (en) | 2012-05-08 | 2012-05-08 | Technique for producing dissolving pulp from whole cotton stalks |
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| CN108797176B (en) * | 2018-06-06 | 2021-02-19 | 华南理工大学 | Method for preparing dissolving pulp from all cotton stalks |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1099501C (en) * | 1999-09-21 | 2003-01-22 | 中国科学院广州化学研究所 | Pulping technology by dissolving eucalyptus |
| CN101381896A (en) * | 2008-10-05 | 2009-03-11 | 山东海龙股份有限公司 | Cotton stalk dissolving pulp and method for making same |
| CN102212974A (en) * | 2011-05-27 | 2011-10-12 | 中国制浆造纸研究院 | Method for producing dissolving pulp |
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