CN108611898B - Method for preparing carboxymethyl fiber by using water medium method and application thereof - Google Patents

Method for preparing carboxymethyl fiber by using water medium method and application thereof Download PDF

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Publication number
CN108611898B
CN108611898B CN201810344964.6A CN201810344964A CN108611898B CN 108611898 B CN108611898 B CN 108611898B CN 201810344964 A CN201810344964 A CN 201810344964A CN 108611898 B CN108611898 B CN 108611898B
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fiber
water
alkali
etherifying agent
dissolving
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CN108611898A (en
Inventor
王建
刘敏
党苗
徐耀威
孙健鹏
邵心怡
刘泽覃
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28023—Fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

Abstract

The invention discloses a method for preparing carboxymethyl fiber by using a water medium method and application thereof, which comprises the steps of dissolving an etherifying agent in water, uniformly mixing plant fibers, soaking at 30-70 ℃ for 1-6 hours to ensure that the etherifying agent is fully contacted with the plant fibers, wherein the mass ratio of the plant fibers to the etherifying agent is 1 (0.1-2), 0.1-2g of the etherifying agent is dissolved in L water of every 3-10m, then dissolving alkali in water to form an alkali solution, adding the alkali solution into the soaked material, carrying out etherification reaction for 1-6 hours at the etherification temperature of 30-90 ℃, wherein the mass ratio of the plant fibers to the alkali is 1 (0.1-2), 0.1-2g of the alkali is dissolved in L water of every 3-10m, and finally washing the reacted product to the pH value of 6-8 to obtain the carboxymethyl fiber.

Description

Method for preparing carboxymethyl fiber by using water medium method and application thereof
Technical Field
The invention relates to the field of heavy metal ion adsorption, in particular to a method for preparing carboxymethyl fiber by using a water medium method and application thereof.
Background
With the rapid development of modern economic society, the amount of urban domestic sewage, industrial and agricultural wastewater and various mining wastewater is continuously increased, and the problem of heavy metal ion pollution of water bodies is increasingly severe. Among methods for treating heavy metal ions in wastewater, the adsorption method has been widely studied and applied due to its advantages of low cost, good effect, strong operability, etc. After the solid adsorbent adsorbs heavy metal ions in the water body, the separation from the water body is easily realized through simple solid-liquid filtration, so that the aim of purifying the water quality is fulfilled. For example: activated carbon, modacrylic fiber, and the like. However, these commonly used adsorbents have some disadvantages during use, such as: activated carbon is used as an adsorption material, and is generally made into a thicker filter layer, so that the water body can realize the adsorption of heavy metal ions through the activated carbon filter layer. After the filter layer is used for a period of time, the filter layer needs to be replaced, the replacement time is long, the workload is large, the price of the activated carbon is expensive, and the reduction of the production cost is not facilitated. When the modified polyacrylonitrile fiber, the modified polyvinyl alcohol fiber and the like are used for adsorbing heavy metal ions, the heavy metal ion adsorbents of the fibers can be directly added into a water body, and are pumped to an inclined net for filtration after the heavy metal ions are adsorbed, so that the solid-liquid separation is realized while the continuous work is realized, but the fibers belong to synthetic fibers, the biodegradability is poor, and the secondary pollution is easy to generate.
Disclosure of Invention
Aiming at the defects of the existing heavy metal ion adsorbing material, the invention provides a method for preparing carboxymethyl fiber by using a water medium method and application thereof, and the carboxymethyl fiber is used for adsorbing heavy metal ions by controlling the etherification substitution degree of plant fiber and keeping the fiber form of the plant fiber while realizing carboxylation of the plant fiber. The environment-friendly adsorption material is realized by fully utilizing the advantages of the operation of the fiber heavy metal ion adsorption material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing carboxymethyl fiber by using an aqueous medium method comprises the following steps:
1) impregnation of raw materials
Dissolving an etherifying agent in water, uniformly mixing the etherifying agent with the plant fiber, soaking for 1-6 hours at the temperature of 30-70 ℃ to ensure that the etherifying agent is fully contacted with the plant fiber, wherein the mass ratio of the plant fiber to the etherifying agent is 1 (0.1-2), and 0.1-2g of the etherifying agent is dissolved in L water of 3-10 m;
2) etherification
Dissolving alkali in water to form alkali liquor, adding the alkali liquor into the soaked material, and carrying out etherification reaction for 1-6h at the etherification temperature of 30-90 ℃, wherein the mass ratio of the plant fiber to the alkali is 1 (0.1-2), and 0.1-2g of alkali is dissolved in L m of water per 3-10m of water;
3) washing machine
Washing the product obtained after the reaction in the step 2) until the pH value is 6-8 to obtain the carboxymethyl fiber.
Furthermore, the plant fiber is needle wood fiber, broad leaf wood fiber, wheat straw fiber or bamboo fiber.
Further, the etherifying agent is sodium chloroacetate or chloroacetic acid.
Further, the alkali is sodium hydroxide, potassium hydroxide or lithium hydroxide.
Further, the prepared carboxymethyl cellulose has an aspect ratio of (100-15): 1.
further, the degree of substitution of the carboxymethyl cellulose prepared is 0.02 to 0.3.
Application of carboxymethyl fiber in heavy metal ion adsorption.
Further, the heavy metal ion is Zn2+。
Compared with the prior art, the invention has the following beneficial technical effects:
the invention keeps the fiber shape by controlling the etherification substitution degree of the plant fiber while realizing the carboxylation of the plant fiber, and the hydroxyl on the cellulose is substituted by carboxyl in the etherification process, thereby increasing the electronegativity of the fiber surface, being beneficial to generating the electrostatic adsorption effect with heavy metal ions with positive charges, simultaneously increasing the aperture and the water retention value of the fiber due to the larger steric hindrance and better water solubility of the carboxyl, enhancing the van der Waals force between the fiber and the heavy metal ions, being more beneficial to generating the physical adsorption effect between the fiber and the heavy metal ions, and in the adsorption test, when the substitution degree of the carboxymethyl fiber reaches 0.28, Zn is added2+The adsorption amount of (B) was 25.64 mg/g. Therefore, the method can be used for the adsorption treatment of heavy metal ions, and realizes the greening of the adsorption material on the basis of fully utilizing the operation advantages of the fiber heavy metal ion adsorption material.
Detailed Description
Embodiments of the invention are described in further detail below:
a method for preparing carboxymethyl fiber by using an aqueous medium method comprises the following steps:
1) impregnation of raw materials
Dissolving an etherifying agent in water, uniformly mixing the etherifying agent with the plant fiber, soaking for 1-6 hours at the temperature of 30-70 ℃ to ensure that the etherifying agent is fully contacted with the plant fiber, wherein the mass ratio of the plant fiber to the etherifying agent is 1 (0.1-2), and 0.1-2g of the etherifying agent is dissolved in L water of 3-10 m;
the plant fiber is one of softwood fiber, hardwood fiber, wheat straw fiber and bamboo fiber, and the etherifying agent is sodium chloroacetate or chloroacetic acid.
2) Etherification
Dissolving alkali in water to form alkali liquor, adding the alkali liquor into the soaked material, and carrying out etherification reaction for 1-6h at the etherification temperature of 30-90 ℃, wherein the mass ratio of the plant fiber to the alkali is 1 (0.1-2), and 0.1-2g of alkali is dissolved in L m of water per 3-10m of water;
the alkali is sodium hydroxide, potassium hydroxide or lithium hydroxide.
3) Washing machine
Washing the product obtained after the reaction in the step 2) until the pH value is 6-8 to obtain carboxymethyl fiber; the aspect ratio of the prepared carboxymethyl fiber is (100-15): 1, the degree of substitution is 0.02-0.3.
The present invention is described in further detail below with reference to examples:
example 1
Weighing 10g of softwood fiber, placing the softwood fiber in a beaker, dissolving 1g of sodium chloroacetate in 30ml of water, uniformly mixing the two, and soaking at 30 ℃ for 6 hours to ensure that the sodium chloroacetate solution is fully contacted with the softwood fiber.
Weighing 1g of sodium hydroxide, dissolving in 30ml of water, adding the sodium hydroxide into the soaked materials, stirring to uniformly mix the sodium hydroxide and the soaked materials, etherifying for 1h at 90 ℃, and washing with water until the pH value is 7 after the reaction is finished to obtain the product. The product has a degree of substitution of 0.08 for Zn2+The amount of adsorbed was 8.10 mg/g.
Example 2
Weighing 10g of hardwood fibers, placing the hardwood fibers in a beaker, dissolving 20g of chloroacetic acid in 100ml of water, uniformly mixing the two, and soaking at 70 ℃ for 1h to ensure that the chloroacetic acid solution is fully contacted with the hardwood fibers.
Weighing 5g of potassium hydroxide, dissolving in 60ml of water, adding the potassium hydroxide into the soaked materials, stirring to uniformly mix the potassium hydroxide and the soaked materials, etherifying for 6 hours at 30 ℃, and washing with water until the pH value is 6 after the reaction is finished to obtain the product. The product has a degree of substitution of 0.18, for Zn2+The amount of adsorbed was 15.08 mg/g.
Example 3
Weighing 10g of wheat straw fiber, placing in a beaker, dissolving 12.5g of sodium chloroacetate in 80ml of water, mixing the two uniformly, and soaking at 60 ℃ for 3h to ensure that the sodium chloroacetate solution is fully contacted with the wheat straw fiber.
Weighing 20g of lithium hydroxide, dissolving the lithium hydroxide in 100ml of water, adding the lithium hydroxide into the soaked materials, stirring to uniformly mix the lithium hydroxide and the soaked materials, etherifying for 2 hours at the temperature of 80 ℃, and washing with water until the pH value is 7 after the reaction is finished to obtain the product. The product has a degree of substitution of 0.21, for Zn2+The amount of adsorbed was 16.96 mg/g.
Example 4
Weighing 10g of bamboo fiber, placing in a beaker, dissolving 12.5g of sodium chloroacetate in 100ml of water, mixing the two uniformly, and soaking at 50 ℃ for 3h to ensure that the sodium chloroacetate solution is fully contacted with the bamboo fiber.
Weighing 7.5g of lithium hydroxide, dissolving in 80ml of water, adding the lithium hydroxide into the soaked materials, stirring to uniformly mix the lithium hydroxide and the soaked materials, etherifying for 4 hours at 80 ℃, and washing with water until the pH value is 8 after the reaction is finished to obtain the product. The product has a degree of substitution of 0.28, for Zn2+The amount of adsorbed was 25.64 mg/g.

Claims (4)

1. A method for preparing carboxymethyl fiber by using an aqueous medium method is characterized by comprising the following steps:
1) impregnation of raw materials
Dissolving an etherifying agent in water, uniformly mixing the etherifying agent with the plant fiber, soaking for 1-6 hours at 30-70 ℃ to ensure that the etherifying agent is fully contacted with the plant fiber, wherein the mass ratio of the plant fiber to the etherifying agent is 1 (0.1-2), and 0.1-2g of the etherifying agent is dissolved in L m of water of every 3-10m, and the etherifying agent is sodium chloroacetate or chloroacetic acid;
2) etherification
Dissolving alkali in water to form alkali liquor, adding the alkali liquor into the soaked material, and carrying out etherification reaction for 1-6h at the etherification temperature of 30-90 ℃, wherein the mass ratio of the plant fiber to the alkali is 1 (0.1-2), and 0.1-2g of alkali is dissolved in L m of water per 3-10m of water;
3) washing machine
Washing the product obtained after the reaction in the step 2) with water until the pH value is 6-8 to obtain the carboxymethyl fiber insoluble in water, wherein the length-width ratio of the prepared carboxymethyl fiber is (100-15): 1, the degree of substitution is 0.02-0.3.
2. The method for preparing carboxymethyl cellulose by using water-borne method as claimed in claim 1, wherein the plant fiber is softwood fiber, hardwood fiber, wheat straw fiber or bamboo fiber.
3. The method for preparing carboxymethyl cellulose by aqueous medium method as claimed in claim 1, wherein the alkali is sodium hydroxide, potassium hydroxide or lithium hydroxide.
4. Use of carboxymethyl cellulose prepared according to any one of claims 1 to 3 for the adsorption of heavy metal ions, wherein the heavy metal ions are Zn2+。
CN201810344964.6A 2018-04-17 2018-04-17 Method for preparing carboxymethyl fiber by using water medium method and application thereof Active CN108611898B (en)

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CN110079327B (en) * 2019-05-30 2021-01-05 北京理工大学 Preparation method and application of straw sodium water retention and conditioning material

Citations (5)

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Publication number Priority date Publication date Assignee Title
CN1490336A (en) * 2002-10-14 2004-04-21 中国科学院成都有机化学研究所 Ultra low viscosity carboxymethyl cellulose and preparing method thereof
CN101830991A (en) * 2010-06-04 2010-09-15 淄博联技化工有限公司 Rapid production technology for carboxymethyl cellulose by aqueous medium process
CN102153663A (en) * 2011-02-22 2011-08-17 玉林师范学院 Method for preparing sodium carboxymethylcellulose with degree of substitution from bagasse
CN103041437A (en) * 2012-12-25 2013-04-17 武汉纺织大学 High-intensity high-hydroscopicity medical dressing containing carboxymethyl cellulose and preparation method thereof
CN103755816A (en) * 2013-12-20 2014-04-30 中国石油大学(北京) Preparation method of sodium carboxymethylcellulose

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US20050002996A1 (en) * 2003-07-02 2005-01-06 Milan Sojka Sustained release compositions and controlled delivery method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1490336A (en) * 2002-10-14 2004-04-21 中国科学院成都有机化学研究所 Ultra low viscosity carboxymethyl cellulose and preparing method thereof
CN101830991A (en) * 2010-06-04 2010-09-15 淄博联技化工有限公司 Rapid production technology for carboxymethyl cellulose by aqueous medium process
CN102153663A (en) * 2011-02-22 2011-08-17 玉林师范学院 Method for preparing sodium carboxymethylcellulose with degree of substitution from bagasse
CN103041437A (en) * 2012-12-25 2013-04-17 武汉纺织大学 High-intensity high-hydroscopicity medical dressing containing carboxymethyl cellulose and preparation method thereof
CN103755816A (en) * 2013-12-20 2014-04-30 中国石油大学(北京) Preparation method of sodium carboxymethylcellulose

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