GB2566234A - Method for preparing multi-functional hydrotalcite/polymer nano-composite auxilliary for leather - Google Patents

Method for preparing multi-functional hydrotalcite/polymer nano-composite auxilliary for leather Download PDF

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Publication number
GB2566234A
GB2566234A GB1900365.6A GB201900365A GB2566234A GB 2566234 A GB2566234 A GB 2566234A GB 201900365 A GB201900365 A GB 201900365A GB 2566234 A GB2566234 A GB 2566234A
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hydrotalcite
water
leather
polymer
functional
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GB201900365D0 (en
GB2566234B (en
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Ma Jianzhong
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/04—Acids; Metal salts or ammonium salts thereof
    • C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C14—SKINS; HIDES; PELTS; LEATHER
    • C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C3/00—Tanning; Compositions for tanning
    • C14C3/02—Chemical tanning
    • C14C3/08—Chemical tanning by organic agents
    • C14C3/22—Chemical tanning by organic agents using polymerisation products
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/46—Polymerisation initiated by wave energy or particle radiation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/46—Polymerisation initiated by wave energy or particle radiation
    • C08F2/56—Polymerisation initiated by wave energy or particle radiation by ultrasonic vibrations
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C14—SKINS; HIDES; PELTS; LEATHER
    • C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C1/00—Chemical treatment prior to tanning
    • C14C1/08—Deliming; Bating; Pickling; Degreasing
    • C—CHEMISTRY; METALLURGY
    • C14—SKINS; HIDES; PELTS; LEATHER
    • C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C11/00—Surface finishing of leather
    • C—CHEMISTRY; METALLURGY
    • C14—SKINS; HIDES; PELTS; LEATHER
    • C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C9/00—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes
    • C14C9/02—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes using fatty or oily materials, e.g. fat liquoring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/267—Magnesium carbonate

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

Provided are a multi-functional hydrotalcite/polymer nano-composite auxiliary for leather and a preparation method therefor, wherein a water-soluble polymer is prepared from acrylic acid and sodium allysulfonate, and hydrotalcite is added and reacted to give the multi-functional hydrotalcite/polymer composite auxiliary.

Description

METHOD FOR PREPARING MULTI-FUNCTIONAL HYDROTALCITE/POLYMER NANO-COMPOSITE AUXILIARY FOR LEATHER
BACKGROUND OF THE INVENTION
1. Technical Field
The present invention relates to pickling and tanning auxiliaries for leather, and more particularly to a multi-functional hydrotalcite/polymer nano-composite auxiliary for leather and a preparation method thereof.
2. Description of Related Art
Polycarboxylic polymers have been extensively used in high exhaustion chrome tanning for leather production. However, the polymers contain too many anions that when leather is combined with an anionic polymer, binding points between anionic chemicals and the collagen structure in leather decrease, which, on one hand, diminishes dye uptake, causing so-called “color failure”, and on the other hand, hinders chemicals such as anionic fatliquor from penetrating and binding leather, thus having adverse effects on the quality of finished leather.
Hydrotalcite materials are layered compounds composed of negatively charged anions (interlayer anions) and positively charged metal hydroxide (the host layer), also known as layered double hydroxides (LDHs). Layered compounds of this type have interlayer anions that are interchangeable, so that various anions may be intercalated between hydrotalcite layers thereby obtaining special functional materials having both properties from the interlayer anions and hydrotalcite host layers. With its electropositivity, a hydrotalcite layer can well adsorb anionic dyes or substances. However, since leather processing is generally performed with water as the medium, application of hydrotalcite in the leather industry is limited by its poor dispersion
-1 properties in water. If hydrotalcite is compound with a water-soluble polymer, not only the dispersion issues of hydrotalcite in water can be solved, but also the “color failure” otherwise seen in use of polymers in leather processing can be prevented, and absorption of other anionic chemicals can be enhanced, thereby contributing to leather products with excellent properties.
SUMMARY OF THE INVENTION
The objective of the present invention is to provide a multifunctional hydrotalcite/polymer nano-composite auxiliary for leather and a preparation method thereof, which not only reduces Cr3+ and Cl' in tanning waste liquor, but also improves dyeing properties and mechanical properties of leather.
For achieving the objective, the present invention discloses:
A method for preparing multi-functional hydrotalcite/polymer nanocomposite auxiliary for leather, being characterized in:
Comprising the following steps:
Step 1: preparing a water-soluble polymer:
placing 45g of acrylic acid, 4.8g of ammonium persulphate, 120g of distilled water in a three-necked flask equipped with a stirrer and a condenser as primers; dissolving 15g of sodium allylsulfonate in 30g of water; when heated to 70°C in a water bath, adding dropwise the solution of sodium allylsulfonate into the three-necked flask over 40min; holding at that temperature and letting reaction run for 5h; cooling; discharging; obtaining the water-soluble polymer;
Step 2: preparing the multi-functional hydrotalcite/polymer nanocomposite auxiliary:
placing 30g of the water-soluble polymer in a three-necked flask;
adding 0.15-0.9g of hydrotalcite; steadily agitating for 2-4h at 40°C;
transferring to an ultrasonic disperser; adjusting the ultrasonic power to 360W-480W; ultrasonically dispersing for 10-50min; discharging; obtaining the multi-functional hydrotalcite/polymer nano-composite auxiliary.
The nano-composite auxiliary prepared using the method for preparing the multi-functional hydrotalcite/polymer nano-composite auxiliary for leather as described previously.
The present invention has the following advantages:
The disclosed multi-functional hydrotalcite/polymer nano-composite auxiliary when added during leather pickling, helps to realize low-saltpickling and low-chromium-tanning production, thereby reducing environmental pollution caused by tanning waste liquor. The auxiliary containing hydrotalcite also helps to improve finished leather in terms of thickening rate and mechanical property. Hydrotalcite exhibits a partially exfoliated and partially intercalated structure in the composite. The positively charged hydrotalcite layers are advantageous for the absorption of anionic dyes and fatliquor in subsequent procedures such as retanning, dyeing, and fatliquoring, thereby improving leather quality. Leather processed using the hydrotalcite/polymer nano-composite auxiliary has color intensity increased by about 20%. The use of the hydrotalcite/polymer nano-composite auxiliary in leather production not only supports the clean development goals of leather tanning agents, but also ensures good quality and improves properties of the finished products.
DETAILED DESCRIPTION OF THE INVENTION
The following description is set forth as below to illustrate the present invention in detail.
-3The method of the multi-functional hydrotalcite/polymer nanocomposite auxiliary for leather according to the present invention is achieved through the following steps:
Step 1: preparing a water-soluble polymer:
placing 45g of acrylic acid, 4.8g of ammonium persulphate, 120g of distilled water in a three-necked flask equipped with a stirrer and a condenser as primers; dissolving 15g of sodium allylsulfonate in 30g of water; when heated to 70°C in a water bath, adding dropwise the solution of sodium allylsulfonate into the three-necked flask over 40min; holding at that temperature and letting reaction run for 5h; cooling; and discharging; obtaining the water-soluble polymer;
Step 2: preparing the multi-functional hydrotalcite/polymer nanocomposite auxiliary:
placing 30g of the water-soluble polymer in a three-necked flask; adding 0.15-0.9g of hydrotalcite; steadily agitating for 2-4h at 40°C; transferring to an ultrasonic disperser; adjusting the ultrasonic power to 360W-480W; ultrasonically dispersing for 10-50min; discharging; obtaining the multi-functional hydrotalcite/polymer nano-composite auxiliary.
Example 1
Placing 45g of acrylic acid, 4.8g of ammonium persulphate, 120g of distilled water in a three-necked flask equipped with a stirrer and a condenser as primers, dissolving 15g of sodium allylsulfonate in 30g of water; when heated to 70°C in a water bath, adding dropwise the sodium allylsulfonate into the three-necked flask over 40min; holding at that temperature and letting reaction run for 5h; cooling; discharging;obtaining the water-soluble polymer. Then 30g of the watersoluble polymer is placed in a three-necked flask, and 0.15g of hydrotalcite is added. Steady agitation is performed at 40°C for 2h. The
-4reactant is transferred to an ultrasonic disperser and ultrasonically dispersed with an ultrasonic power of 360W for lOmin. The produce is discharged and the multi-functional hydrotalcite/polymer nano-composite auxiliary is obtained.
Example 2
45g of acrylic acid, 4.8g of ammonium persulphate, 120g of distilled water are placed in a three-necked flask equipped with a stirrer and a condenser as primers, 15g of sodium allylsulfonate is dissolved in 30g of water; when heated to 70°C in a water bath, the sodium allylsulfonate is added drop wise into the three-necked flask over 40min;the reaction is run for 5h at that temperature; cooling; discharging; the water-soluble polymer is obtained. Then 30g of the water-soluble polymer is placed in a three-necked flask, and 0.45g of hydrotalcite is added. Steady agitation is performed at 40°C for 2.5h. The reactant is transferred to an ultrasonic disperser and ultrasonically dispersed with an ultrasonic power of 360W for 30min. The produce is discharged and the multi-functional hydrotalcite/polymer nano-composite auxiliary is obtained.
Example 3
The method was started with placing 45g of acrylic acid, 4.8g of ammonium persulphate, 120g of distilled water in a three-necked flask equipped with a stirrer and a condenser as primers, dissolving 15g of sodium allylsulfonate in 30g of water; when heated to 70°C in a water bath, adding dropwise the sodium allylsulfonate into the three-necked flask over 40min; holding at that temperature and letting reaction run for 5h; cooling; discharging; obtaining the water-soluble polymer. Then 30g of the water-soluble polymer is placed in a three-necked flask, and 0.75g of hydrotalcite is added. Steady agitation is performed at 40°C for 4h. The reactant is transferred to an ultrasonic disperser and ultrasonically dispersed with an ultrasonic power of 480W for 40min. The produce is
-5discharged and the multi-functional hydrotalcite/polymer nano-composite auxiliary is obtained.
Example 4
Placing 45g of acrylic acid, 4.8g of ammonium persulphate, 120g of distilled water in a three-necked flask equipped with a stirrer and a condenser as primers, dissolving 15g of sodium allylsulfonate in 30g of water; when heated to 70°C in a water bath, adding dropwise sodium allylsulfonate into the three-necked flask over 40min; holding at that temperature and letting reaction run for 5h; cooling; discharging; obtaining the water-soluble polymer. Then placing 30g of the watersoluble polymer in a three-necked flask, and adding 0.9g of hydrotalcite. Steady agitating at 40°C for 4h. Transferring to an ultrasonic disperser and dispersing with an ultrasonic power of 360W for 50min. Discharging and obtaining the multi-functional hydrotalcite/polymer nano-composite auxiliary.
The present invention has been described with reference to the preferred embodiments and it is understood that the embodiments are not intended to limit the scope of the present invention. Moreover, as the contents disclosed herein should be readily understood and can be implemented by a person skilled in the art, all equivalent changes or modifications which do not depart from the concept of the present invention should be encompassed by the appended claims.

Claims (2)

What is claimed is:
1. A method for preparing a multi-functional hydrotalcite/polymer nano-composite auxiliary for leather, being characterized in:
comprising the following steps:
Step 1: preparing a water-soluble polymer:
placing 45g of acrylic acid, 4.8g of ammonium persulphate, 120g of distilled water in a three-necked flask equipped with a stirrer and a condenser as primers; dissolving 15g of sodium allylsulfonate in 30g of water; when heated to 70°C in a water bath, adding dropwise the solution of sodium allylsulfonate into the three-necked flask over 40min; holding at that temperature and letting reaction run for 5h; cooling; discharging; and obtaining the water-soluble polymer;
Step 2: preparing the multi-functional hydrotalcite/polymer nanocomposite auxiliary:
placing 30g of the water-soluble polymer in a three-necked flask; adding 0.15-0.9g of hydrotalcite; steadily agitating for 2-4h at 40°C; transferring to an ultrasonic disperser; adjusting the ultrasonic power to 360W-480W; ultrasonically dispersing for 10-50min; discharging; and obtaining the multi-functional hydrotalcite/polymer nano-composite auxiliary.
2. A nano-composite auxiliary prepared using the method for preparing the multi-functional hydrotalcite/polymer nano-composite auxiliary for leather of claim 1.
GB1900365.6A 2016-06-17 2017-01-17 Method for preparing multi-functional hydrotalcite/polymer nano-composite auxilliary for leather Active GB2566234B (en)

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CN201610429669.1A CN105949369B (en) 2016-06-17 2016-06-17 The preparation method of leather multifunctional water talcum/polymer nanocomposite composite assistant
PCT/CN2017/071369 WO2017215264A1 (en) 2016-06-17 2017-01-17 Method for preparing multi-functional hydrotalcite/polymer nano-composite auxiliary for leather

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CN105949369B (en) * 2016-06-17 2018-06-15 陕西科技大学 The preparation method of leather multifunctional water talcum/polymer nanocomposite composite assistant
CN107881266B (en) * 2017-11-07 2020-05-19 陕西科技大学 In-situ method for preparing layered double-metal hydroxide/polymer nano composite leather retanning agent with deepening effect and method thereof
CN114164308B (en) * 2021-11-18 2023-12-22 陕西科技大学 Multi-carboxyl metal complex tanning agent with self-masking effect and preparation method thereof
CN114369690A (en) * 2022-01-20 2022-04-19 陕西科技大学 Preparation method and tanning method of supermolecular intercalation structure nano tanning agent

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GB201900365D0 (en) 2019-02-27
CN105949369A (en) 2016-09-21
GB2566234B (en) 2021-11-24
WO2017215264A1 (en) 2017-12-21

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