CN110923371B - Environment-friendly wet dyeing and finishing process for preparing original thick high-grade soft sofa leather - Google Patents

Environment-friendly wet dyeing and finishing process for preparing original thick high-grade soft sofa leather Download PDF

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CN110923371B
CN110923371B CN201911093975.2A CN201911093975A CN110923371B CN 110923371 B CN110923371 B CN 110923371B CN 201911093975 A CN201911093975 A CN 201911093975A CN 110923371 B CN110923371 B CN 110923371B
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parts
rotating
agent
softening
tanning agent
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CN110923371A (en
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牛泽
杨义清
孙传基
蔡一雷
温会涛
但卫华
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XINGYE LEATHER TECHNOLOGY CO LTD
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XINGYE LEATHER TECHNOLOGY CO LTD
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    • CCHEMISTRY; METALLURGY
    • C14SKINS; HIDES; PELTS; LEATHER
    • C14CCHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C3/00Tanning; Compositions for tanning
    • C14C3/02Chemical tanning
    • C14C3/08Chemical tanning by organic agents
    • CCHEMISTRY; METALLURGY
    • C14SKINS; HIDES; PELTS; LEATHER
    • C14CCHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C1/00Chemical treatment prior to tanning
    • C14C1/08Deliming; Bating; Pickling; Degreasing
    • CCHEMISTRY; METALLURGY
    • C14SKINS; HIDES; PELTS; LEATHER
    • C14CCHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
    • C14C15/00Apparatus for chemical treatment or washing of hides, skins, or leather

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Treatment And Processing Of Natural Fur Or Leather (AREA)

Abstract

The invention discloses an environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather, which sequentially comprises the following steps of: original blue wet leather batch → water squeezing, shaving, weighing → rinsing → enzyme softening (firstly), water washing → chrome-free retanning → neutralization → enzyme softening (secondly), water washing → dyeing → fat adding → water washing → after finishing; according to the method, the aldehyde tanning agent, the cationic polymer tanning agent and the amphoteric polymer tanning agent are adopted for carrying out chrome-free retanning, the acid protease and the ammonia-free softening enzyme are adopted for carrying out secondary softening treatment, and the neutralization and fatliquoring processes are reasonably matched and designed, so that the prepared original thick high-grade soft sofa leather is soft, full and elastic in body and good in physical and mechanical properties, physical and chemical properties and sensory properties, meets the sofa leather standard, and has good subsequent processing properties; in addition, the process does not adopt materials such as chrome tanning agent, ammonium bicarbonate and the like in the implementation process, and omits the conventional filling procedure, thereby greatly reducing pollution.

Description

Environment-friendly wet dyeing and finishing process for preparing original thick high-grade soft sofa leather
Technical Field
The invention relates to the technical field of leather-making chemistry and leather-making engineering, in particular to an environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather.
Background
The thick sofa leather is a leather product which is very popular in the market all the time, but with the rapid development of social economy and the increasing improvement of the living standard of people, the performance requirements of consumers on the thick sofa leather are higher and higher, including environmental protection, softness and the like. The conventional preparation process of thick sofa leather usually needs retanning by using a chrome tanning agent. Chromium-containing wastewater and chromium-containing sludge generated by chrome retanning are difficult to treat, serious pollution can be caused when the chromium-containing wastewater and the chromium-containing sludge are discharged into the environment, and hexavalent chromium has strong carcinogenicity and can generate great threat to the health of consumers; in addition, the thickness of thick sofa leather often has great influence to the travelling comfort that people sat on the sofa, and the thickness is thicker, and the travelling comfort is higher, but the increase of thickness, the position difference that arouses by each position fibre establishment inconsistent of raw materials skin can be more obvious more, can make sofa leather whole body soft degree reduce and inhomogeneous, especially make former thick sofa (thickness generally surpasss 3mm), and these problems can be more outstanding. Therefore, the development of the environment-friendly wet dyeing and finishing process for preparing the original thick high-grade soft sofa leather has great application prospect.
Disclosure of Invention
The embodiment of the application provides an environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather, and the aldehyde tanning agent, the cationic polymer tanning agent and the amphoteric polymer tanning agent are adopted for carrying out chromium-free retanning, secondary enzyme softening treatment is adopted, and reasonable matching design is carried out on the neutralization process and the fatliquoring process, so that the prepared thick high-grade soft sofa leather is soft, full and elastic in body bone, uniform in whole body and rich in cotton bubble feeling, excellent in softness performance, the problems of low softness, uneven whole body distribution and the like of the thick sofa leather caused by part position difference and large thickness are solved, the process does not adopt chemical materials such as tanning agent and ammonium bicarbonate which have great environmental pollution in the implementation process, the conventional filling process is omitted, the pollution of chromium, ammonia nitrogen, COD (chemical oxygen demand) and the pollution difficulty is greatly reduced.
The embodiment of the application provides an environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather, which sequentially comprises the following steps: original blue wet leather batch → water squeezing, shaving, weighing → rinsing → enzyme softening (firstly), water washing → chrome-free retanning → neutralization → enzyme softening (secondly), water washing → dyeing → fat adding → water washing → after finishing;
the retanning agent adopted in the chrome-free retanning procedure consists of an aldehyde tanning agent, a cationic polymer tanning agent and an amphoteric polymer tanning agent.
Further, the enzyme softening is performed by adopting acid protease, and the enzyme softening is performed by adopting ammonia-free softening enzyme.
Further, the chrome-free retanning process comprises the following specific steps: adding 100 portions of water at 30-35 ℃, 150 portions of aldehyde tanning agent at 2-4 portions and 0.5-1.5 portions of phosphorus-containing fatliquor into the rotary drum, and rotating for 40-60 min; adding 1-2 parts of formic acid, rotating for 60-90min, and adjusting the pH value of the bath liquid to 2.5-3.0; adding 2-5 parts of cationic polymer tanning agent, 1-4 parts of amphoteric polymer tanning agent and 0.5-1.5 parts of cationic fatliquor, and rotating for 90-150 min; adding 1.5-2.5 parts of sodium formate and 0.2-1.2 parts of baking soda, rotating for 60-90min, controlling bath liquid to 3.6-4.0, and discharging liquid.
Further, the neutralization process and the enzyme softening process adopt a one-bath process, and the method comprises the following specific steps: adding 200 parts of water at 30-35 ℃, 2-4 parts of sodium formate and 2-4 parts of neutralizing and retanning agent into the rotary drum, and rotating for 60-90 min; adding 1-3 parts of sodium carbonate and 1-3 parts of liming auxiliary agent, rotating for 90-120min, and controlling the pH value of the bath liquid to 6.0-8.0; adding 0.5-1.5 parts of ammonia-free softening enzyme, rotating for 180min, and discharging liquid.
Further, the dyeing and fatliquoring process adopts a one-bath process, and comprises the following specific steps: adding 50-100 parts of water with the temperature of 30-40 ℃ and 5-8 parts of fatting agent into the rotary drum, and rotating for 60-90 min; adding 1-2 parts of dispersed tannin and 2-4 parts of dye, and rotating for 120-150 min; adding 100-150 parts of hot water at 60-70 ℃, adjusting the temperature of the bath liquid to 50-60 ℃, adding 12-16 parts of fatting agent, and rotating for 90-120 min; adding 1-3 parts of styrene maleic anhydride polymer, and rotating for 30-60 min; adding 2-4 parts of formic acid for 3 times, wherein the interval is 20-30min each time, and adjusting the pH of the bath liquid to 3.5-3.7; adding 0.5-1.5 parts of non-chromium metal tanning agent, rotating for 30-60min, and discharging liquid.
Further, the enzyme softening (i) process comprises the following specific steps: adding water 100-200 parts at 30-40 deg.C and baking soda 0.2-1.2 parts into the rotary drum, rotating for 30-90min, and adjusting the pH of the bath solution to 3.5-4.0; adding 2-5 parts of acid protease, rotating for 180-240min, and discharging liquid.
Further, the rinsing process comprises the following steps: adding 150-250 parts of 35-45 ℃ water, 2-5 parts of oxalic acid, 1-4 parts of industrial salt and 1-2 parts of pickling oil into the rotary drum, rotating for 120-3.0 min, controlling the pH value of the end-point bath liquid to be 2.0-3.0, and draining.
Further, the post-finishing process sequentially includes: wringing and stretching → toggling and drying → hanging and drying → rewetting and standing → shaking and softening → drum milling and softening.
Further, the enzyme activity of the acid protease is 1000-1500 units, and the enzyme activity of the ammonia-free softening enzyme is 500-1000 units.
Further, the fatliquor is at least 3 of polymer fatliquor, synthetic fatliquor, sulfited fatliquor, egg oil fatliquor and mixed fatliquor.
Further, the non-chromium metal tanning agent is one or more of an aluminum tanning agent, a zirconium-aluminum complex tanning agent and a zirconium-aluminum-titanium complex tanning agent.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
1. the invention adopts the aldehyde tanning agent, the cationic polymer tanning agent and the amphoteric polymer tanning agent as the retanning agent for retanning, the aldehyde tanning agent has good dispersion and retanning effects, can promote the penetration and combination of the polymer tanning agent and endow the crust leather with good softness, the cationic polymer tanning agent and the amphoteric polymer tanning agent have good tanning property and filling property, can endow the crust leather with good cotton bubble feeling and promote the absorption of subsequent fatliquoring agents, and the three tanning agents also have synergistic retanning effect, active groups of aldehyde group of the aldehyde tanning agent, cationic group of the cationic polymer tanning agent, amphoteric group of the amphoteric polymer tanning agent and the like can mutually perform cross-linking reaction with amino group and carboxyl group on collagen fiber to form a bigger and empty and loose cross-linking structure between the collagen fiber, endow the crust leather with excellent softening property, and lay a foundation for omitting filling procedures, and chromium-free retanning can greatly reduce chromium pollution and reduce the difficulty of waste liquid treatment.
2. The secondary enzyme softening treatment is adopted, and firstly, the primary enzyme softening is carried out by adopting acid protease with stronger activity after rinsing; after the thick wet blue leather is rinsed by oxalic acid and pickling oil, chromium ions which are not firmly combined and are unevenly combined on the leather surface are removed, a permeation channel of a subsequent material is opened, active groups on collagen fibers are released, and the pickling oil is salt-resistant, acid-resistant and has strong emulsifying capacity, natural oil in the thick wet blue leather can be fully emulsified and dispersed, deeply permeates into the collagen fibers to play a lubricating role, the active groups of the collagen fibers are momentarily closed, the deep permeation and the uniform action of the subsequent material are favorably utilized, the process of enzyme softening is carried out at the moment, and acid protease can rapidly and uniformly permeate into the leather, so that the uniform softening and dispersing effect is achieved on the collagen fibers, and the crust leather is endowed with good softness.
3. The method is characterized in that after the neutralization process, ammonia-free softening enzyme with lower activity is adopted for secondary enzyme softening, the effect of supplementary softening is mainly achieved, sodium carbonate has strong neutralization performance and foamability, the liming auxiliary agent has good fiber expansion dispersion effect, fibers in the leather are fully loosened and separated after neutralization, and enzyme softening is carried out at the moment.
4. The invention directly carries out dyeing and fatliquoring in one bath after enzyme softening finishes, selects the polymer fatliquoring agent and the egg yolk oil fatliquoring agent which have both the fatliquoring function and the filling function, the synthetic fatliquoring agent and the sulfited fatliquoring agent with excellent flexibility, the polymer fatliquoring agent and the mixed fatliquoring agent which are soft and have cotton bubble feeling to carry out fatliquoring, the fatliquoring agent is added for 2 times to be beneficial to infiltration and absorption, part of the fatliquoring agent is added for pre-fatliquoring under the low temperature condition before dyeing, the fat liquoring agent permeates into fibers in leather to play a role of lubrication, the dye is beneficial to deeply permeating and uniformly coloring, the rest fatliquoring agent is added for main fatliquoring under the rising temperature after dyeing, the fatliquoring agent can be rapidly emulsified, infiltrated and uniformly distributed under the high temperature condition, the styrene maleic anhydride polymer is used for further dispersing the fatliquoring agent to promote infiltration, and then formic acid and non-chromium metal tanning agent are used for absorption and fixation in sequence, the fatting agent is gradually absorbed and fixed from the leather to the leather surface, the crust leather is endowed with better fullness, flexibility and cotton foam feeling, the filling process is omitted, and the plant tannin extract, amino resin, acrylic resin, protein filler, synthetic tanning agent and other fillers are not used, so that the chemical materials can be saved, the COD content in the waste liquid is reduced, and the adverse effect of the fillers on the crust leather flexibility and the cotton foam feeling is favorably reduced.
5. The original thick wet blue leather has large thickness and large position difference, and the fibers in the leather are difficult to be uniformly loosened, but the invention adopts aldehyde tanning agent, cationic polymer tanning agent and amphoteric polymer tanning agent to carry out chromium-free retanning, adopts acid protease and ammonia-free softening enzyme to carry out secondary softening treatment, and carries out reasonable collocation design on neutralization and fatliquoring processes, effectively and uniformly loosening and lubricating collagen fibers in the leather, promoting the uniform permeation and action of the material, the prepared thick high-grade soft sofa leather has soft, full and elastic body bones, uniform whole body and rich cotton bubble feeling, excellent soft performance, and all physical and mechanical properties, physical and chemical properties and sensory properties which accord with the sofa leather standard, and has good subsequent processing performance, and solves the problems of reduced softness, uneven whole body distribution and the like caused by large part difference and thickness of the original thick sofa leather.
6. In the implementation process, the invention does not adopt chemical materials with great environmental pollution such as chrome tanning agent, ammonium bicarbonate and the like, omits the conventional filling procedure, can greatly reduce the pollution of chromium, ammonia nitrogen, COD and the like, and reduces the pollution treatment difficulty.
Detailed Description
In order to better understand the technical solutions, the technical solutions will be described in detail below with reference to the embodiments of the specification.
Example 1:
batching original thick blue wet leather: selecting 2 original thick wet blue leathers with consistent producing area, size, thickness and grade;
squeezing, shaving and weighing: the selected 2 original thick blue wet leathers are sequentially squeezed and shaved to a thickness of 3.4-3.5mm, the weight of the shaved original thick blue wet leathers is weighed to 40kg, and the weight parts of reagents used in the subsequent treatment process steps are determined according to the weight;
rinsing: 80kg of water with the temperature of 40 ℃, 1.6kg of oxalic acid (conventional industrial oxalic acid), 1.2kg of industrial salt (conventional industrial salt) and 0.4kg of pickling oil (B1 of Toeplier chemical company) are added into the rotary drum, the rotary drum is rotated for 200min, the pH value of the bath solution at the end point is 2.3-2.4, and water is drained.
Enzyme softening: adding water 50kg at 35 deg.C and baking soda (conventional industrial baking soda) 0.3kg into the rotary drum, rotating for 60min, and adjusting bath solution pH to 3.7-3.8; adding 1.6kg of acid protease (PK-568C of West chemical), rotating for 240min, and discharging.
Washing with water: adding 80kg of water with the temperature of 30 ℃ into the rotary drum, rotating for 10min, and discharging liquid.
Chrome-free retanning: adding 50kg of 32 ℃ water, 1.2kg of aldehyde tanning agent (PF of Sima chemical company) and 0.4kg of phosphorus-containing fatting agent (DB of Toepler chemical company) into a rotary drum, and rotating for 60 min; adding 0.6kg formic acid (conventional industrial formic acid), rotating for 80min, and adjusting bath liquid pH to 2.7-2.8; adding amphoteric polymer tanning agent 2.4kg (cationic polymer tanning agent KCM 1.2kg and amphoteric polymer tanning agent KLS 1.2kg from Kenojing biotechnology company) and cationic fatting agent 0.4kg (GS from Stal chemical company), and rotating for 90-150 min; adding 0.8kg of sodium formate (conventional industrial sodium formate) and 0.35kg of baking soda, rotating for 60min, and discharging liquid when the final bath liquid is 3.7-3.8.
Neutralization and enzyme softening are carried out by adopting a one-bath process: adding 32 deg.C water 60kg, sodium formate 1.2kg, and neutralizing and retanning agent (NG of Drey chemical Co.) 1.6kg into the rotary drum, and rotating for 60 min; adding 0.8kg of sodium carbonate (conventional industrial sodium carbonate) and 0.8kg of liming assistant (AWC of Starer chemical company), rotating for 120min, and regulating bath liquid to 7.0-7.5; 0.35kg of ammonia-free softening enzyme (U5 from Dessel chemical Co.) was added, and the mixture was rotated for 180min to discharge the liquid.
Washing with water: adding 80kg of water with the temperature of 30 ℃ into the rotary drum, rotating for 10min, and discharging liquid.
The dyeing and the fatliquoring adopt a one-bath process: adding 30kg of 35 deg.C water and 2.8kg of fatting agent (polymer fatting agent GS-6061.2kg of Simite chemical company, synthetic fatting agent 94S 0.8kg of Simma chemical company and egg oil fatting agent EY 0.8kg) into the rotary drum, and rotating for 80 min; adding 0.5kg of dispersed tannin (JOM of Shihui chemical company) and 1.2kg of dye (conventional leather dye), and rotating for 140 min; supplementing 60 deg.C hot water 40kg, regulating bath temperature to 55 deg.C, adding 5.6kg of fatting agent (synthetic fatting agent 94S 1.6kg, yolk oil fatting agent EY 1.6kg, sulfited fatting agent MK 1.2kg from Deri chemical company, mixed fatting agent OSL 1.2kg from Toepler chemical company), and rotating for 100 min; adding 0.8kg of styrene maleic anhydride polymer (S of Stahl chemical Co.), and rotating for 40 min; adding 1.2kg formic acid for 3 times at an interval of 25min, and regulating pH to 3.5-3.7; adding 0.3kg of non-chrome metal tanning agent (aluminum tanning agent BN of BASF chemical company), rotating for 60min, and discharging.
Washing with water: adding 80kg of water with the temperature of 30 ℃ into the rotary drum, rotating for 10min, discharging liquid and discharging from the drum.
And (3) after finishing: setting aside, squeezing and stretching → drying of stretching plate → hanging and drying → returning moisture and setting aside → shaking and softening → drum softening.
The above description is only an embodiment utilizing the technical content of the present disclosure, and any modification and variation made by those skilled in the art can be covered by the claims of the present disclosure, and not limited to the embodiments disclosed.

Claims (7)

1. An environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather is characterized by sequentially comprising the following steps of: original blue wet leather batch → water squeezing, shaving, weighing → rinsing → enzyme softening (firstly), water washing → chrome-free retanning → neutralization → enzyme softening (secondly), water washing → dyeing → fat adding → water washing → after finishing;
the chrome-free retanning process comprises the following specific steps: adding 100 portions of water at 30-35 ℃, 150 portions of aldehyde tanning agent at 2-4 portions and 0.5-1.5 portions of phosphorus-containing fatliquor into the rotary drum, and rotating for 40-60 min; adding 1-2 parts of formic acid, rotating for 60-90min, and adjusting the pH value of the bath liquid to 2.5-3.0; adding 2-5 parts of cationic polymer tanning agent, 1-4 parts of amphoteric polymer tanning agent and 0.5-1.5 parts of cationic fatliquor, and rotating for 90-150 min; adding 1.5-2.5 parts of sodium formate and 0.2-1.2 parts of baking soda, rotating for 60-90min, controlling the pH value of the bath liquid to 3.6-4.0, and discharging liquid;
the enzyme softening step comprises the following specific steps: adding water 100-200 parts at 30-40 deg.C and baking soda 0.2-1.2 parts into the rotary drum, rotating for 30-90min, and adjusting the pH of the bath solution to 3.5-4.0; adding 2-5 parts of acid protease, rotating for 180-;
the neutralization process and the enzyme softening process adopt a one-bath process, and the method comprises the following specific steps: adding 200 parts of water at 30-35 ℃, 2-4 parts of sodium formate and 2-4 parts of neutralizing and retanning agent into the rotary drum, and rotating for 60-90 min; adding 1-3 parts of sodium carbonate and 1-3 parts of liming auxiliary agent, rotating for 90-120min, and controlling the pH value of the bath liquid to 6.0-8.0; adding 0.5-1.5 parts of ammonia-free softening enzyme, rotating for 180min, and discharging liquid.
2. The environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather according to claim 1, characterized in that the dyeing and fatliquoring processes adopt a one-bath process, and the specific steps are as follows: adding 50-100 parts of water with the temperature of 30-40 ℃ and 5-8 parts of fatting agent into the rotary drum, and rotating for 60-90 min; adding 1-2 parts of dispersed tannin and 2-4 parts of dye, and rotating for 120-150 min; adding 100-150 parts of hot water at 60-70 ℃, adjusting the temperature of the bath liquid to 50-60 ℃, adding 12-16 parts of fatting agent, and rotating for 90-120 min; adding 1-3 parts of styrene maleic anhydride polymer, and rotating for 30-60 min; adding 2-4 parts of formic acid for 3 times, wherein the interval is 20-30min each time, and adjusting the pH value of the bath liquid to 3.5-3.7; adding 0.5-1.5 parts of non-chromium metal tanning agent, rotating for 30-60min, and discharging liquid.
3. The environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather according to claim 1, characterized in that the rinsing process comprises the following steps: adding 150-250 parts of 35-45 ℃ water, 2-5 parts of oxalic acid, 1-4 parts of industrial salt and 1-2 parts of pickling oil into the rotary drum, rotating for 120-3.0 min, controlling the pH value of the end-point bath liquid to be 2.0-3.0, and draining.
4. The environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather according to claim 1, characterized in that the after-finishing process comprises the following steps in sequence: setting aside, squeezing and stretching → drying of stretching plate → hanging and drying → returning moisture and setting aside → shaking and softening → drum softening.
5. The environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather as claimed in claim 1, wherein the enzyme activity of the acid protease is 1000-1500 units, and the enzyme activity of the ammonia-free softening enzyme is 500-1000 units.
6. The environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather according to claim 2, wherein the fatliquoring agent is at least 3 of polymer fatliquoring agent, synthetic fatliquoring agent, sulfited fatliquoring agent, egg oil fatliquoring agent and mixed fatliquoring agent.
7. The environment-friendly wet dyeing and finishing process for preparing thick high-grade soft sofa leather according to claim 2, characterized in that the non-chromium metal tanning agent is one or more of aluminum tanning agent, zirconium-aluminum complex tanning agent and zirconium-aluminum-titanium complex tanning agent.
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