CN107237197B - A kind of wood dissolving pulp deashing agent and process for deashing - Google Patents

A kind of wood dissolving pulp deashing agent and process for deashing Download PDF

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Publication number
CN107237197B
CN107237197B CN201710597684.1A CN201710597684A CN107237197B CN 107237197 B CN107237197 B CN 107237197B CN 201710597684 A CN201710597684 A CN 201710597684A CN 107237197 B CN107237197 B CN 107237197B
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China
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dissolving pulp
deashing
wooden
acidizer
polybag
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CN201710597684.1A
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CN107237197A (en
Inventor
吴朝军
于冬梅
李书平
李荣刚
王代启
欧阳志周
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Qilu University of Technology
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Qilu University of Technology
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The present invention relates to the wooden dissolving pulp preparing technical field, more particularly to a kind of wooden dissolving pulp deashing agent, including bleeding agent, mixing acidizer and chelating agent.The wooden dissolving pulp process for deashing:Infiltration is handled;Mixed acid processing;Chelation treatment.The gap of the wooden dissolving pulp fiber finer cell wall and the interfacial tension at pit after floating are reduced by the bleeding agent in deashing agent, mixing acidizer and chelating agent are added again, chelate transitional metal ion, it is acidified silicate ion and generates silicic acid precipitation, idetified separation is carried out to silicate ion and transition metal ions, since sour dosage is low, the reduction of cellulosic degree of polymerization in the wooden dissolving pulp is avoided, to improve the removal rate of ash content and the reduction amplitude for reducing the wooden dissolving pulp average degree of polymerization in the wooden dissolving pulp.Technological process is simple, chemicals clean environment firendly used.

Description

A kind of wood dissolving pulp deashing agent and process for deashing
Technical field
The present invention relates to the wooden dissolving pulp preparing technical field, more particularly to it is molten to further relate to wood for a kind of wooden dissolving pulp deashing agent Solve the process for deashing of slurry.
Background technology
Dissolving pulp mainly as synthetic cotton, acetate fiber, enteric solubility coated tablet and medical artificial kidney etc. raw material, One of the important source material of the industry such as modern light, spinning, medicine, chemical industry, military project is become.Currently, in the world to the need of dissolving pulp The amount of asking is growing day by day, and dissolving pulp requires high content of cellulose, low hemicellulose, lignin, extract and content of ashes.
Ash content refers to residue of the dissolving pulp in 725 DEG C of Muffle furnaces after calcination, it be mainly silica and calcium, magnesium, Copper, iron plasma, ash content height can make viscose filtration difficult, while iron, the copper plasma in ash content can accelerate alkali cellulose aging It degrades, aging technique is caused to fluctuate, or even have an effect on viscose fiber strength and color and luster.The wooden dissolving pulp user is to ash content in dissolving pulp Content has strict demand, and according to quality difference, content of ashes requires to be respectively to be less than 0.10%(725℃)With less than 0.12%(725 ℃).
Dissolving pulp mainly is prepared using timber such as poplar, Eucalyptus, Acacia, pines both at home and abroad, ash content in these raw materials For content because place of production difference difference is larger, content is generally 0.3~0.9%, the inorganic brought into along with boiling and bleaching process Chemicals, content of ashes increases to 1.0% or so in the wooden dissolving pulp after bleaching, this cannot be satisfied the wooden dissolving pulp user to dissolving pulp The requirement of middle content of ashes.
In order to reduce the ash content of dissolving pulp, dissolving pulp manufacturing enterprise will carry out sour processing after association with pulp bleaching, generally at acid It is relatively low to manage pH value control(PH=1-3), the time is longer (1-3 hours), and low pH value processing environment easily makes few fibers in dissolving pulp Element occurs acidic hydrolysis and drops poly-, and the average degree of polymerization of dissolving pulp can reduce, this not only influences the reactivity worth of dissolving pulp, can also Increase the washing water consumption of dissolving pulp after acid is handled.This technique is extremely difficult to 80% to the wooden dissolving pulp ash content removal rate after drift, wood It is more than 5% that the average degree of polymerization of dissolving pulp, which reduces amplitude,.If it is efficient and to the average degree of polymerization of the wooden dissolving pulp to explore ash disposal Small technology is influenced, it will be of great advantage to the wooden dissolving pulp manufacturing enterprise.
Invention content
Low in order to solve ash content removal rate in the above dissolving pulp, existing ash content minimizing technology is to dissolving pulp average degree of polymerization Big problem is influenced, it is high that this application discloses ash content removal rates in a kind of dissolving pulp, is influenced on dissolving pulp average degree of polymerization small The wooden dissolving pulp deashing agent.
Disclosed herein as well is a kind of wooden dissolving pulp process for deashing.
It is reduced after drift in the wooden dissolving pulp at fibrocyte parietal suture gap and pit by means of the bleeding agent in deashing agent first Interfacial tension, by adsorption and diffusion chelating agent so far and hydrogen radical ion pair remain in the transition metal at gap and pit from Son is chelated, and so that it is converted into silicic acid the progress acid modification of the silicate ion of remaining and be precipitated, and since sour dosage is low, is kept away The reduction of cellulosic degree of polymerization in the wooden dissolving pulp is exempted from.After this process, the wooden dissolving pulp ash content removal rate is more than after drift 90%, the average degree of polymerization of the wooden dissolving pulp reduces amplitude and is less than 2%.
The present invention is achieved by the following measures:
A kind of wood dissolving pulp deashing agent, including bleeding agent, mixing acidizer and chelating agent, wherein
Bleeding agent is thermally coupled distillation columns, neopelex, OP-13 and OP-15 mass ratioes 2: 2:1:1 mixture;
Mixing acidizer is H2SO4, HCl and HAC mass ratioes be 2:2:1 mixture;
Chelating agent is EDETATE SODIUM and calgon mass ratio is 20:1 mixture.
A kind of wood dissolving pulp process for deashing, includes the following steps:
(1)Infiltration is handled:The wooden dissolving pulp is added in plastic sealing bag after floating, and bleeding agent is added, additive amount is oven dry stock The 0.006-0.06% of quality, after being rubbed 1-5 minutes with hand, polybag is put into 20-40 DEG C of constant temperature by sealed plastic bag, when processing Between 5-20min;
(2)Mixed acid processing:Mixing acidizer is added to by step(1)The wooden dissolving pulp after penetrant treating In, mixing acidizer additive amount is the 0.25-1.5% of oven dry stock quality, after hand rubbing polybag 1-5 minutes, is moulded in sealing Material bag, then polybag is put into 20-40 DEG C of constant temperature, processing time is 10-20 min;
(3)Chelation treatment:Chelating agent is added to by step(2)It mixes acidizer treated in the wooden dissolving pulp, Amount of chelant is the 0.021-0.21% of oven dry stock quality, after hand rubbing polybag 1-5 minutes, polybag in sealing, then will Polybag is put into 20-40 DEG C of constant temperature, and processing time is 20-40 min, is washed till neutrality.
The wooden dissolving pulp process for deashing, preferred steps(1)It is middle to adjust a concentration of 5-10% of the wooden dissolving pulp with distilled water.
The wooden dissolving pulp process for deashing, preferred steps(1)Middle bleeding agent additive amount is the 0.02- of oven dry stock quality 0.04%。
The wooden dissolving pulp process for deashing, preferred steps(2)Middle mixing acidizer additive amount is oven dry stock quality 0.7-0.9%。
The wooden dissolving pulp process for deashing, preferred steps(3)Middle amount of chelant is the 0.09- of oven dry stock quality 0.11%。
The wooden dissolving pulp process for deashing, the preferably wooden dissolving pulp is poplar slab dissolving pulp, bamboo willow dissolving pulp or Eucalyptus Dissolving pulp.
It is analyzed by People's Republic of China (PRC) textile industry standard FZ/T 50010.3-2011 and FZ/T 50010.5-1998 The degree of polymerization and content of ashes of the wooden dissolving pulp of test.
The beneficial effects of the invention are as follows:
(1)It is reduced after drift at the gap of the wooden dissolving pulp fiber finer cell wall and pit by bleeding agent in deashing agent first Interfacial tension, then mixing acidizer and chelating agent are added, chelate transitional metal ion is acidified silicate ion and generates silicic acid Precipitation carries out idetified separation to silicate ion and transition metal ions and avoids fiber in the wooden dissolving pulp since sour dosage is low The reduction of the plain degree of polymerization, to improve the removal rate of ash content and the drop for reducing the wooden dissolving pulp average degree of polymerization in the wooden dissolving pulp Low amplitude.
(2)Using process wood dissolving pulp of the present invention, technological process is simple, chemicals clean environment firendly used.
Specific implementation mode
In order to better understand the present invention, it is further illustrated with reference to specific example.
Embodiment 1:
Poplar slab dissolving pulp after floating is handled using present invention process, the average degree of polymerization of poplar slab dissolving pulp is 490, Whiteness 81%ISO, content of ashes 0.77%.
Step 1 is:Over dry poplar slab dissolving pulp 15g is taken, it is 0.02% that bleeding agent, which optimizes dosage, is adjusted with distilled water Slurry concentration is 8%, and after being rubbed 1 minute with hand, polybag is put into constant temperature water bath, controls water bath with thermostatic control by sealed plastic bag Bath temperature degree T=30 DEG C, processing time are 10 min;
Step 2 is:It will mix in the wooden dissolving pulp after acidizer is added to penetrant treating, mixing acidizer is excellent It is 0.9% to change dosage, after hand rubbing polybag 1 minute, polybag in sealing, then polybag is put into constant temperature water bath, it controls Constant temperature water bath temperature processed T=30 DEG C, processing time are 15 min;
Step 3 is:Chelating agent is added to mixing acidizer treated in the wooden dissolving pulp, chelating agent optimizes dosage It is 0.09%, after hand rubbing polybag 1 minute, polybag in sealing, then polybag is put into constant temperature water bath, control constant temperature Water bath temperature T=30 DEG C, processing time are that 30 min. are washed to filtrate with distillation and are in neutrality after chelating agent processing.By above-mentioned After process, the average degree of polymerization of poplar slab dissolving pulp is 488, whiteness 83%ISO, content of ashes 0.04%.
After this process, poplar slab dissolving pulp ash content index can fully meet user and contain to ash content in dissolving pulp The requirement of amount.
Embodiment 2:
Bamboo willow dissolving pulp after floating is handled using present invention process, the average degree of polymerization of bamboo willow dissolving pulp is 513, whiteness 85% ISO, content of ashes 0.87%.
Step 1 is:Over dry bamboo willow dissolving pulp 15g is taken, it is 0.03% that bleeding agent, which optimizes dosage, and it is dense to adjust slurry with distilled water Degree is 8%, and after being rubbed 1 minute with hand, polybag is put into constant temperature water bath, control constant temperature water bath temperature T by sealed plastic bag =30 DEG C, processing time is 10 min;
Step 2 is:It will mix in the wooden dissolving pulp after acidizer is added to penetrant treating, mixing acidizer is excellent It is 0.8% to change dosage, after hand rubbing polybag 1 minute, polybag in sealing, then polybag is put into constant temperature water bath, it controls Constant temperature water bath temperature processed T=30 DEG C, processing time are 15 min;
Step 3 is:Chelating agent is added to mixing acidizer treated in the wooden dissolving pulp, chelating agent optimizes dosage It is 0.10%, after hand rubbing polybag 1 minute, polybag in sealing, then polybag is put into constant temperature water bath, control constant temperature Water bath temperature T=30 DEG C, processing time are that 30 min. are washed to filtrate with distillation and are in neutrality after chelating agent processing.By above-mentioned After process, the average degree of polymerization of bamboo willow dissolving pulp is 510, whiteness 87%ISO, content of ashes 0.05%.
After this process, bamboo willow dissolving pulp ash content index can fully meet user to content of ashes in dissolving pulp It is required that.
Embodiment 3:
Eucalyptus dissolving pulp after floating is handled using present invention process, the average degree of polymerization of eucalyptus dissolving pulp is 713, whiteness 86% ISO, content of ashes 0.57%.
Step 1 is:Over dry eucalyptus dissolving pulp 15g is taken, it is 0.04% that bleeding agent, which optimizes dosage, and slurry is adjusted with distilled water A concentration of 8%, after being rubbed 1 minute with hand, polybag is put into constant temperature water bath, controls water bath with thermostatic control bath temperature by sealed plastic bag T=30 DEG C are spent, processing time is 10 min;
Step 2 is:It will mix in the wooden dissolving pulp after acidizer is added to penetrant treating, mixing acidizer is excellent It is 0.7% to change dosage, after hand rubbing polybag 1 minute, polybag in sealing, then polybag is put into constant temperature water bath, it controls Constant temperature water bath temperature processed T=30 DEG C, processing time are 15 min;
Step 3 is:Chelating agent is added to mixing acidizer treated in the wooden dissolving pulp, chelating agent optimizes dosage It is 0.11%, after hand rubbing polybag 1 minute, polybag in sealing, then polybag is put into constant temperature water bath, control constant temperature Water bath temperature T=30 DEG C, processing time are that 30 min. are washed to filtrate with distillation and are in neutrality after chelating agent processing.By above-mentioned After process, the average degree of polymerization of eucalyptus dissolving pulp is 713, whiteness 88%ISO, content of ashes 0.03%.
After this process, eucalyptus dissolving pulp ash content index can fully meet user to content of ashes in dissolving pulp It is required that.
Embodiment 4:
Compared with example 1, the penetrant treating operation in step 1 is omitted, remaining operation is identical with embodiment 1, as a result For:The average degree of polymerization of poplar slab dissolving pulp is 488, whiteness 83%ISO, content of ashes 0.14%.
After this process, poplar slab dissolving pulp ash content index cannot meet user to content of ashes in dissolving pulp Requirement.
Embodiment 5:
Compared with example 1, the mixed acid processing operation in step 2 is omitted, remaining operation is identical with embodiment 1, as a result For:The average degree of polymerization of poplar slab dissolving pulp is 490, whiteness 81%ISO, content of ashes 0.16%.
After this process, poplar slab dissolving pulp ash content index cannot meet user to content of ashes in dissolving pulp Requirement.
Embodiment 6:
Compared with example 1, the chelating agent operation processing step in step 3 is omitted, remaining operation is identical with embodiment 1, As a result it is:The average degree of polymerization of poplar slab dissolving pulp is 487, whiteness 81%ISO, content of ashes 0.15%.
After this process, poplar slab dissolving pulp ash content index cannot meet user to content of ashes in dissolving pulp Requirement.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not limited by embodiment System, other any changes made without departing from the spirit and principles of the present invention, modification, combination, replacement, simplification should be Equivalence replacement mode, is included within the scope of the present invention.

Claims (8)

1. a kind of wood dissolving pulp deashing agent, it is characterised in that including bleeding agent, mixing acidizer and chelating agent, wherein
Bleeding agent is thermally coupled distillation columns, neopelex, OP-13 and OP-15 mass ratioes 2:2:1:1 Mixture;
Mixing acidizer is H2SO4, HCl and HAc mass ratioes be 2:2:1 mixture;
Chelating agent is EDETATE SODIUM and calgon mass ratio is 20:1 mixture.
2. a kind of wood dissolving pulp process for deashing, it is characterised in that include the following steps:
(1)Infiltration is handled:The wooden dissolving pulp is added in plastic sealing bag after floating, and the bleeding agent described in claim 1 is added, adds Dosage is the 0.006-0.06% of oven dry stock quality, and after being rubbed 1-5 minutes with hand, polybag is put into constant temperature by sealed plastic bag 20-40 DEG C, processing time 5-20min;
(2)Mixed acid processing:Mixing acidizer described in claim 1 is added to by step(1)Penetrant treating In the wooden dissolving pulp afterwards, mixing acidizer additive amount is the 0.25-1.5% of oven dry stock quality, is divided with hand rubbing polybag 1-5 Zhong Hou, polybag in sealing, then polybag is put into 20-40 DEG C of constant temperature, processing time is 10-20 min;
(3)Chelation treatment:Chelating agent described in claim 1 is added to by step(2)After mixing acidizer processing The wooden dissolving pulp in, amount of chelant is the 0.021-0.21% of oven dry stock quality, after hand rubbing polybag 1-5 minute, is sealed Upper polybag, then polybag is put into 20-40 DEG C of constant temperature, processing time is 20-40 min, is washed till neutrality.
3. wood dissolving pulp process for deashing according to claim 2, it is characterised in that step(1)It is middle molten with distilled water adjusting wood Solution starches a concentration of 5-10%.
4. wood dissolving pulp process for deashing according to claim 2, it is characterised in that step(1)Middle bleeding agent additive amount is exhausted The 0.02-0.04% of dry pulp quality.
5. wood dissolving pulp process for deashing according to claim 2, it is characterised in that step(2)Middle mixing acidizer addition Amount is the 0.7-0.9% of oven dry stock quality.
6. wood dissolving pulp process for deashing according to claim 2, it is characterised in that step(3)Middle amount of chelant is over dry Starch the 0.09-0.11% of quality.
7. wood dissolving pulp process for deashing according to claim 2, it is characterised in that the wooden dissolving pulp be poplar slab dissolving pulp, Bamboo willow dissolving pulp or eucalyptus dissolving pulp.
8. wood dissolving pulp process for deashing according to claim 2, it is characterised in that step(1)Middle bleeding agent additive amount is exhausted The 0.03% of dry pulp quality, step(2)Middle mixing acidizer additive amount is the 0.8% of oven dry stock quality, step(3)Middle chelating agent Dosage is the 0.10% of oven dry stock quality.
CN201710597684.1A 2017-07-21 2017-07-21 A kind of wood dissolving pulp deashing agent and process for deashing Expired - Fee Related CN107237197B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111636101B (en) * 2020-04-24 2022-01-14 赛得利(九江)纤维有限公司 Method for removing metal ions in waste cotton fabric dissolving pulp

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Publication number Priority date Publication date Assignee Title
US6706143B1 (en) * 1996-03-19 2004-03-16 International Paper Company Minimizing chlorinated organics in pulp bleaching processes
CN101748631A (en) * 2009-12-18 2010-06-23 华南理工大学 Efficient and clean puling and bleaching method dissolving alpha-pulp by Chinese alpine rush
CN102108646A (en) * 2010-12-17 2011-06-29 山东轻工业学院 Process for purifying dissolving pulp
CN102277762A (en) * 2011-09-02 2011-12-14 山东轻工业学院 Process for producing dissolving pulp by utilizing bleaching wood pulp board
CN103382671A (en) * 2013-07-29 2013-11-06 四川理工学院 Clean pulping technology for high-polymerization-degree bamboo pulp
CN103726377A (en) * 2014-01-21 2014-04-16 四川理工学院 Clean pulping method for low-polymerization degree bamboo pulp

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6706143B1 (en) * 1996-03-19 2004-03-16 International Paper Company Minimizing chlorinated organics in pulp bleaching processes
CN101748631A (en) * 2009-12-18 2010-06-23 华南理工大学 Efficient and clean puling and bleaching method dissolving alpha-pulp by Chinese alpine rush
CN102108646A (en) * 2010-12-17 2011-06-29 山东轻工业学院 Process for purifying dissolving pulp
CN102277762A (en) * 2011-09-02 2011-12-14 山东轻工业学院 Process for producing dissolving pulp by utilizing bleaching wood pulp board
CN103382671A (en) * 2013-07-29 2013-11-06 四川理工学院 Clean pulping technology for high-polymerization-degree bamboo pulp
CN103726377A (en) * 2014-01-21 2014-04-16 四川理工学院 Clean pulping method for low-polymerization degree bamboo pulp

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