CN109989115B - Ramie cold rolling stacking oxygen bleaching degumming process - Google Patents

Ramie cold rolling stacking oxygen bleaching degumming process Download PDF

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Publication number
CN109989115B
CN109989115B CN201910350250.0A CN201910350250A CN109989115B CN 109989115 B CN109989115 B CN 109989115B CN 201910350250 A CN201910350250 A CN 201910350250A CN 109989115 B CN109989115 B CN 109989115B
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ramie
concentration
degumming
oxygen bleaching
stabilizer
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CN109989115A (en
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张小祝
别晓东
杨继前
李文成
王惠
廖光辉
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Sichuan Jb Ramie Co ltd
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Sichuan Jb Ramie Co ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01CCHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
    • D01C1/00Treatment of vegetable material
    • D01C1/02Treatment of vegetable material by chemical methods to obtain bast fibres

Abstract

The invention belongs to the technical field of ramie fiber preparation. Provides a ramie cold rolling and stacking oxygen bleaching degumming process. The process comprises the following steps: (1) the first cold pad-batch oxygen bleaching pretreatment: mixing raw ramie with a degumming scouring agent, performing dipping pretreatment, and washing to obtain pretreated ramie; the degumming boiling agent comprises the following raw materials: the first hydrogen peroxide, the first sodium hydroxide and an oxygen bleaching stabilizer; the raw materials of the pretreated working solution comprise: a non-silicone bleaching stabilizer, second hydrogen peroxide, second sodium hydroxide and a high-efficiency penetrant; (2) second boiling: adding third sodium hydroxide into the pretreated ramie, boiling and scouring, and beating the ramie to obtain refined dry ramie; (3) and (4) pickling and oil feeding. The degumming process not only can ensure that the ramie has high degumming yield, the degumming wastewater is easy to treat, the prepared ramie fibers have high strength, low residual gum and good extensibility, but also has simple bleaching steps and good bleaching effect, silicon scale cannot be formed on equipment, and the quality of the obtained ramie fibers is improved.

Description

Ramie cold rolling stacking oxygen bleaching degumming process
Technical Field
The invention belongs to the technical field of ramie fiber preparation, and particularly relates to a ramie cold rolling pad-batch oxygen bleaching degumming process.
Background
The traditional ramie degumming process comprises unpacking of raw ramie, bundling, caging, pickling, washing, boiling for the first time, washing, boiling for the second time, beating, bleaching and pickling, dehydrating and shaking, feeding oil, deoiling, shaking and drying.
The degumming and boiling-off are divided into two-stage boiling-off (first boiling-off and second boiling-off), the NaoH consumption in the working procedure is large, the steam consumption in the boiling-off working procedure is large, the pH value, the BOD value and the COD value of the degumming waste water are high, and the degumming waste water is not easy to treat. Degumming, bleaching and pickling also include bleaching, peracid and water washing. According to the traditional process, the bleaching process is carried out by acid and water washing, so that the steps are complicated, the bleaching effect is poor, and the fibers are easily damaged in the bleaching process to destroy the fiber quality.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the ramie cold rolling pad-batch oxygen bleaching degumming process, which can improve the ramie degumming production efficiency, ensure that the prepared ramie fibers have high strength and good elongation, ensure that degumming wastewater is easy to treat, ensure that the bleaching step is simple and the bleaching effect is good, prevent silicon scale from forming on equipment and improve the quality of the ramie fibers.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
a ramie cold rolling stacking oxygen bleaching degumming process comprises the following steps: (1) first cold rolling stack oxygen bleaching pretreatment: mixing raw ramie with a degumming boiling agent according to a mass ratio of 100: 1.5-3.0, dipping and pretreating for 24-48h at normal temperature, and washing to obtain pretreated ramie; the degumming boiling agent comprises the following raw materials: first hydrogen peroxide water with the concentration of 8-12g/L, first sodium hydroxide with the concentration of 6-12g/L and an oxygen bleaching stabilizer with the concentration of 9-11 g/L; the pretreated oxygen bleaching working solution comprises the following raw materials: a non-silica bleaching stabilizer with the concentration of 9-11g/L, second hydrogen peroxide with the concentration of 8-12g/L, second sodium hydroxide with the concentration of 10-12g/L and a high-efficiency penetrating agent with the concentration of 2-3 g/L; (2) second boiling: adding 4-6g/L third sodium hydroxide into the pretreated ramie, boiling at 95-100 ℃ for 1.5-2h, and beating to obtain washed ramie; (3) acid washing and oil feeding: immersing the washed refined dry ramie into H with the concentration of 0.5-1.0g/L2SO4Soaking in the working solution at normal temperature for 5-10min, washing with water until the pH value of the washing reaches 6-7, applying oil, and drying to obtain refined dry ramie.
The invention has the beneficial effects that:
the ramie cold rolling pad-batch oxygen bleaching degumming process provided by the invention comprises the improvement of a degumming scouring agent formula and the improvement of process parameters in the scouring process, so that the ramie degumming is more thorough and the strong elongation of the prepared ramie fiber can be ensured; the bleaching is carried out by adopting the cold pad-batch oxygen bleaching, and according to the formula of the adopted oxygen bleaching working solution and the improvement of the oxygen bleaching process, the bleaching step is simple, the bleaching effect is good, no silica scale is formed on equipment, and the quality of the obtained ramie fiber is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The ramie cold pad-batch oxygen bleaching degumming process provided by the embodiment of the invention is specifically explained below.
A ramie cold rolling and stacking oxygen bleaching degumming process comprises acid leaching: the ramie raw ramie is soaked in concentrated sulfuric acid with the concentration of 1.5ml/L for 1h at the bath ratio of 1:20 and the temperature of 60 ℃. By adopting the acid leaching of the steps, partial water-soluble substances, hydrolyzed pectin and hemicellulose in the raw ramie can be effectively removed, so that the boiling burden is reduced, the boiling effect is improved, the boiling color is improved, and the ramie fibers achieve the purposes of white color and soft hand feeling and loose fibers.
(1) First cold rolling stack oxygen bleaching pretreatment: mixing raw ramie with a degumming boiling agent according to a mass ratio of 100: 1.5-3.0, dipping and pretreating for 24-48h at normal temperature, and washing to obtain pretreated ramie; the degumming boiling agent comprises the following raw materials: first hydrogen peroxide water with the concentration of 8-12g/L, first sodium hydroxide with the concentration of 6-12g/L and an oxygen bleaching stabilizer with the concentration of 9-11 g/L; wherein the oxygen bleaching stabilizer comprises one of HP-SI and rare earth stabilizer.
The oxygen bleaching stabilizer is used as an environment-friendly metal ion chelating agent, has the characteristics of good compatibility, strong chelating capacity, wide application environment and the like, and can effectively replace the traditional non-degradable chelating agent. The oxygen bleaching stabilizer, hydrogen peroxide and sodium hydroxide are cooperatively matched according to the proportion, so that the effects of improving the ramie degumming production efficiency, reducing the wastewater treatment difficulty, improving the strength and the extensibility of ramie fibers and the like can be further achieved.
Wherein, the raw materials of the pretreated oxygen bleaching working solution comprise: a non-silica bleaching stabilizer with the concentration of 9-11g/L, second hydrogen peroxide with the concentration of 8-12g/L, second sodium hydroxide with the concentration of 10-12g/L and a high-efficiency penetrating agent with the concentration of 2-3 g/L. Furthermore, the concentration of the non-silica bleaching stabilizer is 10g/L, the concentration of the second hydrogen peroxide is 10g/L, the concentration of the second sodium hydroxide is 11g/L, and the concentration of the high-efficiency penetrant is 2 g/L. According to the proportion of the raw materials of the oxygen bleaching working solution, the ramie fiber with good whiteness can be obtained, the formation of silica scale on equipment can be avoided, and the quality of the ramie fiber is improved.
Further, in this example, the non-silicone bleach stabilizers include the non-silicone stabilizer AR-750 and the non-silicone stabilizer XF-01. Wherein, the non-silicon stabilizer AR-750 has stronger adsorption and chelation effects on metal ions, is alkali-resistant and high-temperature-resistant, and has better stability; the non-silicon stabilizer XF-01 has excellent performance, less consumption and low cost. In this example, the mass ratio of the non-silicon stabilizer AR-750 to the non-silicon stabilizer XF-01 was 1:0.2 to 0.5. The non-silica bleaching stabilizer adopting the proportion can effectively reduce or inhibit the over-rapid decomposition of hydrogen peroxide, reduce the waste of hydrogen peroxide and obviously improve the whiteness and capillary effect of the fiber.
(2) Second boiling: adding 4-6g/L third sodium hydroxide into the pretreated ramie, boiling at 95-100 ℃ for 1.5-2h, and beating to obtain washed ramie refined dry ramie.
(3) Acid washing and oil feeding: immersing the washed refined dry ramie into H with the concentration of 0.5-1.0g/L2SO4Soaking in the working solution at normal temperature for 5-10min, washing with water until the pH value of the washing reaches 6-7, applying oil, and drying to obtain refined dry ramie.
In this embodiment, the water washing includes: washing with water at 85-88 deg.C for 7min, at 58-62 deg.C for 5min, and at 22-27 deg.C for 3 min. The gradient water washing is beneficial to more thorough washing.
It should be noted that, the traditional process is to perform secondary scouring on the acid-leached raw ramie, and according to the improvement of the two scouring processes, the difference of chemical structures and properties of cellulose and non-cellulose is utilized to enable most non-cellulose substances in the raw ramie to undergo complex chemical changes of dissolution, cracking, saponification and emulsification under the actions of the degumming scouring agent of the first cold pad-batch oxygen bleaching pretreatment and the sodium hydroxide of the second scouring, so that the glue and impurities are removed, and the pure ramie fiber is obtained.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a ramie cold rolling pad-batch oxygen bleaching degumming process, which comprises the following steps:
(1) first cold rolling stack oxygen bleaching pretreatment: mixing raw ramie with a degumming boiling agent according to a mass ratio of 100: 1.5, mixing, dipping and pretreating for 24 hours at normal temperature, and washing to obtain pretreated ramie; the degumming boiling agent comprises the following raw materials: first hydrogen peroxide water with the concentration of 8g/L, first sodium hydroxide with the concentration of 6g/L and HP-SI with the concentration of 9 g/L; the pretreated oxygen bleaching working solution comprises the following raw materials: a non-silica bleaching stabilizer with the concentration of 10g/L, second hydrogen peroxide with the concentration of 10g/L, second sodium hydroxide with the concentration of 11g/L and a high-efficiency penetrating agent with the concentration of 2 g/L; the non-silicone bleaching stabilizer comprises AR-750 and XF-01 in a mass ratio of 1: 0.2.
(2) Second boiling: adding third sodium hydroxide with the concentration of 4g/L into the pretreated ramie, boiling for 2 hours at 95 ℃, and beating and drying the ramie to obtain the washed ramie.
(3) Acid washing and oil feeding: immersing the washed refined and dried ramie into H with the concentration of 0.5g/L2SO4Soaking in the working solution at normal temperature for 10min, washing with water until the pH value of the washing reaches 6-7, applying oil, and drying to obtain refined dry ramie.
Example 2
The embodiment provides a ramie cold rolling pad-batch oxygen bleaching degumming process, which comprises the following steps:
(1) first cold rolling stack oxygen bleaching pretreatment: mixing raw ramie with a degumming boiling agent according to a mass ratio of 100: 3.0, dipping and pretreating for 48 hours at normal temperature, and washing to obtain pretreated ramie; the degumming boiling agent comprises the following raw materials: first hydrogen peroxide water with the concentration of 12g/L, first sodium hydroxide with the concentration of 12g/L and HP-SI with the concentration of 11 g/L; the pretreated oxygen bleaching working solution comprises the following raw materials: a non-silica bleaching stabilizer with the concentration of 10g/L, second hydrogen peroxide with the concentration of 10g/L, second sodium hydroxide with the concentration of 11g/L and a high-efficiency penetrating agent with the concentration of 2 g/L; the non-silicone bleaching stabilizer comprises AR-750 and XF-01 in a mass ratio of 1: 0.2.
(2) Second boiling: adding third sodium hydroxide with the concentration of 4g/L into the pretreated ramie, boiling for 2 hours at 95 ℃, and beating and drying the ramie to obtain the washed ramie.
(3) Acid washing and oil feeding: immersing the washed refined and dried ramie into H with the concentration of 0.5g/L2SO4Soaking in the working solution at room temperature for 10min, and washing with water to obtain water solutionAnd after the pH value reaches 6-7, oiling and drying to obtain the ramie refined dry ramie.
Example 3
The embodiment provides a ramie cold rolling pad-batch oxygen bleaching degumming process, which comprises the following steps:
(1) first cold rolling stack oxygen bleaching pretreatment: mixing raw ramie with a degumming boiling agent according to a mass ratio of 100: 2.0, dipping and pretreating for 30 hours at normal temperature, and washing to obtain pretreated ramie; the degumming boiling agent comprises the following raw materials: first hydrogen peroxide water with the concentration of 10g/L, first sodium hydroxide with the concentration of 8g/L and HP-SI with the concentration of 10 g/L; the pretreated oxygen bleaching working solution comprises the following raw materials: a non-silica bleaching stabilizer with the concentration of 10g/L, second hydrogen peroxide with the concentration of 10g/L, second sodium hydroxide with the concentration of 11g/L and a high-efficiency penetrating agent with the concentration of 2 g/L; the non-silicone bleaching stabilizer comprises AR-750 and XF-01 in a mass ratio of 1: 0.2.
(2) Second boiling: adding third sodium hydroxide with the concentration of 4g/L into the pretreated ramie, boiling for 2 hours at 95 ℃, and beating and drying the ramie to obtain the washed ramie.
(3) Acid washing and oil feeding: immersing the washed refined and dried ramie into H with the concentration of 0.5g/L2SO4Soaking in the working solution at normal temperature for 10min, washing with water until the pH value of the washing reaches 6-7, applying oil, and drying to obtain refined dry ramie.
Example 4
The embodiment provides a ramie cold rolling pad-batch oxygen bleaching degumming process, which comprises the following steps:
(1) first cold rolling stack oxygen bleaching pretreatment: mixing raw ramie with a degumming boiling agent according to a mass ratio of 100: 2.0, dipping and pretreating for 30 hours at normal temperature, and washing to obtain pretreated ramie; the degumming boiling agent comprises the following raw materials: first hydrogen peroxide water with the concentration of 10g/L, first sodium hydroxide with the concentration of 8g/L and rare earth stabilizer with the concentration of 10 g/L; the pretreated oxygen bleaching working solution comprises the following raw materials: a non-silica bleaching stabilizer with the concentration of 9g/L, second hydrogen peroxide with the concentration of 8g/L, second sodium hydroxide with the concentration of 10g/L and a high-efficiency penetrating agent with the concentration of 2 g/L; the non-silicone bleaching stabilizer comprises AR-750 and XF-01 in a mass ratio of 1: 0.2.
(2) Second boiling: adding third sodium hydroxide with the concentration of 6g/L into the pretreated ramie, boiling at 100 ℃ for 1.5h, and beating and drying the ramie to obtain washed ramie;
(3) acid washing and oil feeding: immersing the washed refined and dried ramie into H with the concentration of 1g/L2SO4Soaking in the working solution at normal temperature for 5min, washing with water until the pH value of the washing reaches 6-7, applying oil, and drying to obtain refined dry ramie.
Example 5
The embodiment provides a ramie cold rolling pad-batch oxygen bleaching degumming process, which comprises the following steps:
(1) first cold rolling stack oxygen bleaching pretreatment: mixing raw ramie with a degumming boiling agent according to a mass ratio of 100: 2.0, dipping and pretreating for 30 hours at normal temperature, and washing to obtain pretreated ramie; the degumming boiling agent comprises the following raw materials: first hydrogen peroxide water with the concentration of 10g/L, first sodium hydroxide with the concentration of 8g/L and rare earth stabilizer with the concentration of 10 g/L; the pretreated oxygen bleaching working solution comprises the following raw materials: a non-silica bleaching stabilizer with the concentration of 11g/L, second hydrogen peroxide with the concentration of 12g/L, second sodium hydroxide with the concentration of 12g/L and a high-efficiency penetrating agent with the concentration of 3 g/L; the non-silicone bleaching stabilizer comprises AR-750 and XF-01 in a mass ratio of 1: 0.5.
(2) Second boiling: adding third sodium hydroxide with the concentration of 5g/L into the pretreated ramie, boiling at 98 ℃ for 1.8h, and beating and drying the ramie to obtain washed ramie;
(3) acid washing and oil feeding: immersing the washed refined and dried ramie into H with the concentration of 0.8g/L2SO4Soaking in the working solution at normal temperature for 8min, washing with water until the pH value of the washing reaches 6-7, applying oil, and drying to obtain refined dry ramie.
Experimental example 1
The ramie fibers prepared in examples 1 to 5 were set as test groups 1 to 5; the degumming rates of the ramie fibers provided by the experimental groups 1 to 5 (degumming rate (weight of the raw ramie before degumming-weight of the ramie fibers after degumming)/weight of the raw ramie before degumming) were respectively detected; respectively detecting the whiteness of the ramie fibers provided by the experimental groups 1-5 by using a whiteness tester; detecting the breaking strength of the ramie fibers provided by the experimental groups 1-5 by using an electronic fabric strength tester; the results are shown in Table 1:
TABLE 1
Figure GDA0003024211810000081
Figure GDA0003024211810000091
As can be seen from the data in Table 1, the ramie fibers prepared by the cold pad-batch oxygen bleaching degumming process for ramie provided by the embodiment of the invention have high degumming rate, good whiteness and excellent tensile property.
In conclusion, the ramie cold rolling and stacking oxygen bleaching degumming process provided by the invention has the advantages of high ramie degumming yield, low pH of degumming waste water, good treatment and the like.
The prepared ramie refined dry ramie has high strength, good extensibility, simple bleaching step and good bleaching effect, and can not form silica scale on equipment, thereby improving the quality of the obtained ramie fiber.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A ramie cold rolling heap oxygen bleaching degumming process is characterized in that: the method comprises the following steps:
(1) first cold rolling stack oxygen bleaching pretreatment: mixing raw ramie with a degumming boiling agent according to a mass ratio of 100: 1.5-3.0, dipping and pretreating for 24-48h at normal temperature, and washing to obtain pretreated ramie; the degumming scouring agent comprises the following raw materials: first hydrogen peroxide water with the concentration of 8-12g/L, first sodium hydroxide with the concentration of 6-12g/L and an oxygen bleaching stabilizer with the concentration of 9-11 g/L; the pretreated oxygen bleaching working solution comprises the following raw materials: a non-silica bleaching stabilizer with the concentration of 9-11g/L, second hydrogen peroxide with the concentration of 8-12g/L, second sodium hydroxide with the concentration of 10-12g/L and a high-efficiency penetrating agent with the concentration of 2-3 g/L;
(2) second boiling: adding 4-6g/L third sodium hydroxide into the pretreated ramie, boiling at 95-100 ℃ for 1.5-2h, and beating to obtain washed ramie;
(3) acid washing and oil feeding: immersing the washed refined and dried ramie into H with the concentration of 0.5-1.0g/L2SO4Soaking in the working solution at normal temperature for 5-10min, washing with water until the pH value of the washing reaches 6-7, applying oil, and drying to obtain refined dry ramie.
2. The ramie cold rolling pad-batch oxygen bleaching degumming process according to claim 1, characterized in that: in the step (1), the non-silicon oxygen bleaching stabilizer comprises a non-silicon stabilizer AR-750 and a non-silicon stabilizer XF-01; the mass ratio of the non-silicon stabilizer AR-750 to the non-silicon stabilizer XF-01 is 1: 0.2-0.5.
3. The ramie cold rolling pad-batch oxygen bleaching degumming process according to claim 1, characterized in that: the oxygen bleaching stabilizer comprises one of HP-SI and rare earth stabilizer.
4. The ramie cold rolling pad-batch oxygen bleaching degumming process according to claim 1, characterized in that: in the step (1), the concentration of the non-silica bleaching stabilizer is 10g/L, the concentration of the second hydrogen peroxide is 10g/L, the concentration of the second sodium hydroxide is 11g/L, and the concentration of the high-efficiency penetrating agent is 2 g/L.
5. The ramie cold rolling pad-batch oxygen bleaching degumming process according to claim 1, characterized in that: in the step (3), the water washing comprises water washing at 85-88 ℃ for 7min, water washing at 58-62 ℃ for 5min and water washing at 22-27 ℃ for 3min in sequence.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997005219A1 (en) * 1995-07-26 1997-02-13 Röhm Gmbh Vegetable oil enzymatic degumming process by means of aspergillus phospholipase
CN101012575A (en) * 2007-02-02 2007-08-08 重庆市涪陵金帝工业集团有限公司 Ramee degumming process
CN101096773A (en) * 2006-06-26 2008-01-02 湖南苎麻技术研究中心 Energy-saving environment-friendly type china grass degumming process

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997005219A1 (en) * 1995-07-26 1997-02-13 Röhm Gmbh Vegetable oil enzymatic degumming process by means of aspergillus phospholipase
CN101096773A (en) * 2006-06-26 2008-01-02 湖南苎麻技术研究中心 Energy-saving environment-friendly type china grass degumming process
CN101012575A (en) * 2007-02-02 2007-08-08 重庆市涪陵金帝工业集团有限公司 Ramee degumming process

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