CN109797256B - Processing technology of cow leather and tanning agent for cow leather - Google Patents
Processing technology of cow leather and tanning agent for cow leather Download PDFInfo
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- CN109797256B CN109797256B CN201910122834.2A CN201910122834A CN109797256B CN 109797256 B CN109797256 B CN 109797256B CN 201910122834 A CN201910122834 A CN 201910122834A CN 109797256 B CN109797256 B CN 109797256B
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Abstract
The invention relates to a processing technology of cow leather and a tanning agent for cow leather, belonging to the technical field of leather processing. The invention has the advantages of excellent leather performance, less chromium consumption and less environmental pollution. The tanning agent adopted by the invention is safe and environment-friendly, and has the advantages of being capable of being respectively combined with collagen fibers and chromium powder on the surface of cow leather and improving the utilization rate of chromium.
Description
Technical Field
The invention relates to the technical field of leather processing, in particular to a processing technology of cow leather and a tanning agent for cow leather.
Background
The leather is animal leather which is obtained by physical and chemical processing such as unhairing, tanning and the like and is denatured and not easy to rot, is formed by tightly weaving natural protein fibers in a three-dimensional space, has a special grain layer on the surface, has natural grains and luster, and is comfortable in hand feeling. The tanning step of the process for preparing the cow leather is the most critical process stage, and the tanning of the cow hide adopts a tanning agent, so that the tanning agent is combined with hide protein (collagen) and is converted into leather. At present, tanning agents for processing leather are mainly divided into plant tanning agents, mineral tanning agents and organic tanning agents, wherein the mineral tanning agents mainly comprise chromium salts and aluminum salts, the mineral tanning agents are used for producing light leather such as clothes and bags, and the technology for producing the leather by adopting a chrome tanning method accounts for most of the processes. However, in the traditional chrome tanning process, the absorption rate of the chrome tanning agent is only about sixty percent, a large amount of the chrome tanning agent remains in the tanning waste liquid, and the direct discharge of the chrome-containing waste liquid can cause serious pollution to soil and water. Meanwhile, because of the shortage of chromium resources in China, the leather is prepared by adopting a chrome tanning process, and a chrome tanning agent needs to be imported, so that the production cost of the leather is higher.
In the prior art, patent application with publication number CN107419040A discloses a tanning agent for cowhide and a cowhide tanning process, wherein the tanning agent comprises methacrylic acid, resorcinol, urea formaldehyde, azone, dibutyl itaconate, bis-carboxyethylamine, sodium phthalate, o-carboxybenzaldehyde, di-n-butylamine, fatty aldehyde and maleic acid, and the tanning agent does not contain chromium, but the tanned wet-heat resistance stability, physical and mechanical properties, softness and other properties are not as good as those of chrome tanned leather. The development of less chrome tanning aids to achieve the superior performance of chrome tanned leathers is a focus and focus of research in this field.
Disclosure of Invention
Aiming at the defects in the prior art, the first purpose of the invention is to provide a processing technology of cowhide leather, which has the advantages of excellent leather performance, less chromium consumption and less environmental pollution.
A second object of the present invention is to provide a tanning agent for bovine hide, which has advantages of being capable of binding with collagen fibers and chromium powder on the surface of bovine hide, respectively, and improving the utilization rate of chromium.
In order to achieve the first object, the invention provides the following technical scheme: a processing technology of cow leather comprises the following steps:
pretreatment of tanning: comprises the steps of cleaning, unhairing, degreasing and softening the raw cowhide, and obtaining the cowhide to be tanned after the treatment.
Tanning: pre-tanning cowhide to be tanned by adopting a polymer-based nano composite tanning agent, then adding formic acid and chromium powder, and tanning under the environment of pH 4 to obtain a semi-finished product.
Fat liquoring: and (3) putting the semi-finished product into water at the temperature of 50-60 ℃, adding ammonia water for treatment for 15-30 min, and then adding a fatting agent for treatment for 60-90 min to obtain the finished product.
The polymer-based nano-composite tanning agent is a polymer-based silicon dioxide nano-composite tanning agent.
By adopting the technical scheme, the raw cowhide is subjected to cleaning, unhairing, degreasing and softening treatment before tanning, wherein the cleaning is to remove dirt on the raw cowhide and dissolve soluble protein in the raw cowhide in water. The dehairing is to remove the skin and hair needles of raw cowhide to expose the grain surface, so that the surface of the cowhide is smooth and beautiful, and the degreasing is to remove a large amount of lipid contained in the cowhide to avoid affecting the quality of finished leather. Softening is to remove the scale on the cowhide and dissolve part of the skin protein, so that the finished leather is soft. Then tanning the cow leather by adopting a polymer-based nano-composite tanning agent and chromium powder, wherein the polymer-based nano-composite tanning agent is a polymer-based silicon dioxide nano-composite tanning agent, nano-silicon dioxide has a unique three-dimensional silica structure, the surfaces of particles are rich in hydroxyl groups, the surface energy is high, and after being compounded with a polymer, the wet-heat resistance stability, the physical and mechanical properties, the thermal stability and the weather resistance of leather can be improved, the using amount of chromium powder is reduced, the utilization rate of the chromium powder in the tanning process is increased, the reduction of the chromium content in tanning waste liquid is facilitated, and the pollution to the environment is reduced. The tanned leather is fatted to make the leather plump and soft, improve the strength, reduce the fold lines and reduce the hygroscopicity.
The method is further set that in the pre-tanning process, the using amount of the polymer-based nano composite tanning agent is 12-16% of the mass of the cow leather to be tanned, and the pre-tanning time is 4.5-7 h.
By adopting the technical scheme, the dosage and the time of the composite tanning agent can influence the tanning effect, the tanning agent pre-tanning and the chromium powder tanning of the invention are carried out in the environment with the pH value of 4, and the composite tanning agent with the dosage has the best tanning effect on the cow leather, and the tanned leather has better performances in the aspects of shrinkage temperature, thickening rate and the like.
The tanning method is further set to be characterized in that in the tanning process, the addition amount of formic acid is 0.2-0.3% of the mass of the cow leather to be tanned, the addition amount of chromium powder is 0.3-0.5% of the mass of the cow leather to be tanned, and the tanning time after the formic acid and the chromium powder are added is 3-4 hours.
By adopting the technical scheme, the cow leather is processed according to the addition amount and the tanning time, and the polymer-based nano composite tanning agent is coordinated with chromium ions to form a collagen-tanning agent-chromium network structure, so that the stability of the collagen structure is improved, the utilization rate of chromium powder is improved, and the residual chromium content in the tanning waste liquid is reduced.
The invention is further configured that the polymer-based nanocomposite tanning agent is prepared from the following raw materials in parts by weight: 0.1-0.3 part of lignosulfonate, 0.5-1.5 parts of polyaspartic acid, 0.5-1.5 parts of tetraethyl silicate and 20-30 parts of acrylic resin.
By adopting the technical scheme, the polymer-based nano composite tanning agent prepared from lignosulfonate, polyaspartic acid, tetraethyl silicate and acrylic resin can be combined with collagen in multiple points. Meanwhile, the functional group contained in the composite tanning agent can be complexed with chromium to form a complex, so that the chromium has higher fixation rate on the cowhide through the interaction between the composite tanning agent and the leather collagen fiber as well as between the chromium complex and the leather collagen fiber.
The invention further provides that the polymer-based nanocomposite tanning agent is prepared according to the following method: mixing lignosulfonate, absolute ethyl alcohol and ammonia water, performing ultrasonic dispersion, dropwise adding tetraethyl silicate at 50-65 ℃, stirring for 8-12 hours at 50-65 ℃, performing centrifugal separation, and collecting a filter cake; mixing the filter cake with polyaspartic acid and deionized water, stirring for 20-22 h at the pH of 3.5-4.5 and the temperature of 60-70 ℃, performing centrifugal separation again, mixing the separated solid with acrylic resin, performing ultrasonic dispersion, and stirring for 2-3 h to obtain the product.
By adopting the technical scheme, the lignosulfonate is firstly reacted with tetraethyl silicate to generate a lignosulfonate and nano silicon dioxide compound, then the compound is reacted with the polyaspartic acid, and the generated product is mixed with acrylic resin to obtain the composite tanning agent.
The invention further provides that the fatliquor is at least two of fish oil fatliquor, lecithin fatliquor or synthetic fatliquor.
In order to achieve the second object, the invention provides the following technical scheme: a tanning agent for cow leather is prepared from the following raw materials in parts by weight: 0.1-0.3 part of lignosulfonate, 0.5-1.5 parts of polyaspartic acid, 0.5-1.5 parts of tetraethyl silicate and 20-30 parts of acrylic resin. Further, the tanning agent is prepared according to the following method: mixing lignosulfonate, absolute ethyl alcohol and ammonia water, performing ultrasonic dispersion, dropwise adding tetraethyl silicate at 50-65 ℃, stirring for 8-12 hours at 50-65 ℃, performing centrifugal separation, and collecting a filter cake; mixing the filter cake with polyaspartic acid and deionized water, stirring for 20-22 h at the pH of 3.5-4.5 and the temperature of 60-70 ℃, performing centrifugal separation again, mixing the separated solid with acrylic resin, performing ultrasonic dispersion, and stirring for 2-3 h to obtain the product.
By adopting the technical scheme, the tanning agent prepared according to the formula and the method can combine collagen fibers and chromium ions of cowhide, so that chromium is favorably fixed, the utilization rate of the chromium is improved, and the stability of the collagen fibers on the cowhide is favorably improved.
In conclusion, the beneficial technical effects of the invention are as follows:
firstly, pretanning cow leather by adopting a polymer-based nano composite tanning agent, and then adding chromium powder for tanning, a network structure is formed among collagen fibers, the composite tanning agent and chromium ions on the cow leather, so that the stability of the collagen structure is favorably improved, the absorption rate of the chromium ions can be improved, and the content of chromium sesquioxide in waste liquid is reduced.
In the polymer-based nano composite tanning agent, the lignosulfonate contains carboxyl which can react with chromium to form a complex, and the lignosulfonate and the polyaspartic acid can improve the particle size distribution of the nano silicon dioxide, improve the dispersibility of the nano silicon dioxide, enable the nano silicon dioxide to permeate into pores of leather, effectively fill in collagen fibers and be beneficial to improving the tanning effect of the nano silicon dioxide.
Detailed Description
The following describes a technical solution of an embodiment of the present invention.
Examples
Example one
This example provides a tanning agent for bovine hide, prepared as follows: 0.04kg of lignosulfonate, 5L of absolute ethanol and 0.35L of ammonia water are uniformly mixed, ultrasonically dispersed, 0.214L of tetraethyl silicate is added dropwise at 50 ℃, the temperature is maintained, stirring is carried out for 8 hours, the stirred reaction solution is subjected to centrifugal separation, and a filter cake is collected. Mixing the filter cake with 0.2kg of aspartic acid and 3.75L of deionized water, stirring for 20h at the temperature of 60 ℃ and the pH of 3.5, centrifuging again, mixing the separated solid with 8kg of acrylic resin, performing ultrasonic dispersion, and stirring for 2h to obtain the product.
Example two
The difference between the present embodiment and the first embodiment is mainly as follows: the tanning agent of this example was prepared as follows: 0.12kg of lignosulfonate, 12L of absolute ethyl alcohol and 0.9L of ammonia water are uniformly mixed, ultrasonically dispersed, 0.6L of tetraethyl silicate is added dropwise at 65 ℃, the temperature is maintained, stirring is carried out for 12 hours, the stirred reaction solution is subjected to centrifugal separation, and a filter cake is collected. Mixing the filter cake with 0.6kg of aspartic acid and 10L of deionized water, stirring for 22h at the temperature of 70 ℃ and the pH value of 4.5, centrifuging again, mixing the separated solid with 12kg of acrylic resin, performing ultrasonic dispersion, and stirring for 3h to obtain the product.
EXAMPLE III
The difference between the present embodiment and the first embodiment is mainly as follows: the tanning agent of this example was prepared as follows: 0.08kg of lignosulfonate, 8L of absolute ethyl alcohol and 0.6L of ammonia water are uniformly mixed, ultrasonically dispersed, 0.4L of tetraethyl silicate is added dropwise at 58 ℃, the temperature is maintained, stirring is carried out for 10 hours, the stirred reaction solution is subjected to centrifugal separation, and a filter cake is collected. Mixing the filter cake with 0.4kg of aspartic acid and 6.5L of deionized water, stirring for 21h at the temperature of 65 ℃ and the pH value of 4, centrifuging again, mixing the separated solid with 10kg of acrylic resin, performing ultrasonic dispersion, and stirring for 2.5h to obtain the product.
Example four
The embodiment provides a processing technology of cow leather, which comprises the following steps:
pretreatment of tanning: taking 50kg of raw cowhide, cleaning the surface of the raw cowhide, putting the cleaned raw cowhide in 50kg of water, adding 25g of fatty alcohol-polyoxyethylene ether and 20g of ferrous sulfate into the water, adding 0.5kg of triethanolamine after rotating for 1.5h, adding 1.75kg of sodium hydroxide after continuously rotating for 10min, adding 3kg of hydrogen peroxide after rotating for 15min, and rotating for 3 h. And then taking out the cowhide and soaking the cowhide in 100kg of water, adding 1.5kg of degreasing agent at 36 ℃, washing the cowhide clean with warm water after rotating for 90min, softening the cowhide under the action of softening enzyme, and rotating the cowhide in the softening enzyme for 75min to obtain the cowhide to be tanned.
Tanning: putting the cowhide to be tanned in 60kg of water, adding 6kg of polymer-based nano-composite tanning agent, rotating for 7 hours, adding 0.1kg of formic acid and 0.15kg of chromium powder, and tanning for 3 hours under the environment of pH 4 to obtain a semi-finished product, wherein the polymer-based nano-composite tanning agent adopted in the embodiment is the product prepared in the first embodiment.
Fat liquoring: and (3) putting the semi-finished product into water with the temperature of 50 ℃, adding ammonia water for treatment for 15min, then adding the fish oil fatliquor and the synthetic fatliquor, and treating for 60min to obtain the fish oil fatliquor.
EXAMPLE five
The present embodiment is different from the fourth embodiment mainly in that: tanning in the processing technology of the embodiment is to place the cowhide to be tanned in 60kg of water, add 8kg of polymer-based nano-composite tanning agent, rotate for 4.5 hours, then add 0.15kg of formic acid and 0.25kg of chromium powder, tan for 4 hours in the environment of pH 4 to prepare a semi-finished product, and the polymer-based nano-composite tanning agent adopted in the embodiment is the product prepared in the embodiment two.
EXAMPLE six
The present embodiment is different from the fourth embodiment mainly in that: tanning in the processing technology of the embodiment is to place the cowhide to be tanned in 60kg of water, add 7kg of polymer-based nano-composite tanning agent, rotate for 5.5 hours, then add 0.125kg of formic acid and 0.2kg of chromium powder, tan for 3.5 hours in the environment of pH 4 to prepare a semi-finished product, and the polymer-based nano-composite tanning agent adopted in the embodiment is the product prepared in the third embodiment.
Comparative example
Comparative example 1
The comparative example differs from the fourth example mainly in that: the tanning of the comparative example adopts a chromium tanning agent, and the dosage of the chromium tanning agent is 12 kg.
Comparative example No. two
The comparative example differs from the fourth example mainly in that: the tanning of the comparative example adopts plant tanning agent, and is tannin extract purchased from the chemical industry of Ezetimol. Performance test
The leather produced in the fourth to sixth examples and the first and second comparative examples was tested according to the national standard leather for furniture (GB/T16799-2008), and the appearance defects, tearing force and abrasion resistance of the product were tested, and the content of chromium sesquioxide in the tanning waste liquid was tested in each comparative example and in the fourth to sixth examples, and the test results are shown in Table 1.
TABLE 1 test results of examples four to six and comparative examples one and two
| Group of | Appearance of the product | Tear force/N | Abrasion resistance (CS-10,1000g,500r) | Chromium oxide content (mg/L) |
| Example four | Defect free | 48 | No obvious damage and peeling | 172 |
| EXAMPLE five | Defect free | 42 | No obvious damage and peeling | 176 |
| EXAMPLE six | Defect free | 45 | No obvious damage and peeling | 168 |
| Comparative example 1 | Defect free | 43 | No obvious damage and peeling | 2380 |
| Comparative example No. two | Defect free | 22 | The surface of the steel plate is cracked and slightly peeled | 0 |
As can be seen from Table 1, the leathers prepared by the fourth to sixth examples of the invention and the first and second comparative examples have no obvious defects in appearance, and the leathers prepared by the fourth to sixth examples of the invention are similar to the first comparative example in tearing force and wear resistance, namely, the leathers prepared by the invention are equivalent to the leathers prepared by a chrome tanning method in mechanical property, while the chromium sesquioxide content in the waste water produced by the tanning of the invention is obviously reduced, which proves that the waste water produced by the processing technology of the invention is more environment-friendly. The tanning of the comparative example two is also environment-friendly, and the waste water does not contain chromium, but the prepared leather is far inferior to the leather prepared by the invention or the leather prepared by the chromium tanning method in terms of mechanical properties.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (6)
1. The processing technology of the cow leather is characterized by comprising the following steps:
pretreatment of tanning: cleaning, unhairing, degreasing and softening the raw cowhide to obtain the cowhide to be tanned;
tanning: pre-tanning cowhide to be tanned by adopting a polymer-based nano composite tanning agent, then adding formic acid and chromium powder, and tanning under the environment of pH 4 to prepare a semi-finished product;
fat liquoring: putting the semi-finished product into water at the temperature of 50-60 ℃, adding ammonia water for treatment for 15-30 min, and then adding a fatting agent for treatment for 60-90 min to obtain the finished product;
the polymer-based nano composite tanning agent is polymer-based silicon dioxide nano composite tanning agent and is prepared from the following raw materials in parts by weight: 0.1-0.3 part of lignosulfonate, 0.5-1.5 parts of polyaspartic acid, 0.5-1.5 parts of tetraethyl silicate and 20-30 parts of acrylic resin;
the polymer-based nanocomposite tanning agent is prepared according to the following method: mixing lignosulfonate, absolute ethyl alcohol and ammonia water, performing ultrasonic dispersion, dropwise adding tetraethyl silicate at 50-65 ℃, stirring for 8-12 hours at 50-65 ℃, performing centrifugal separation, and collecting a filter cake; mixing the filter cake with polyaspartic acid and deionized water, stirring for 20-22 h at the pH of 3.5-4.5 and the temperature of 60-70 ℃, performing centrifugal separation again, mixing the separated solid with acrylic resin, performing ultrasonic dispersion, and stirring for 2-3 h to obtain the product.
2. The processing technology of the cow leather according to claim 1, wherein in the pretanning process, the using amount of the polymer-based nano composite tanning agent is 12-16% of the mass of the cow leather to be tanned, and the pretanning time is 4.5-7 h.
3. The processing technology of the cow leather as claimed in claim 1, wherein in the tanning process, the addition amount of formic acid is 0.2-0.3% of the mass of the cow leather to be tanned, the addition amount of chromium powder is 0.3-0.5% of the mass of the cow leather to be tanned, and the tanning time after the formic acid and the chromium powder are added is 3-4 h.
4. The process for processing cowhide leather according to claim 1, wherein the fatliquor is at least two of fish oil fatliquor, lecithin fatliquor or synthetic fatliquor.
5. A tanning agent for cowhide, characterized in that the tanning agent is a polymer-based nanocomposite tanning agent according to any one of claims 1 to 4, the tanning agent is prepared from the following raw materials in parts by weight: 0.1-0.3 part of lignosulfonate, 0.5-1.5 parts of polyaspartic acid, 0.5-1.5 parts of tetraethyl silicate and 20-30 parts of acrylic resin.
6. A tanning agent for bovine skins as claimed in claim 5, characterized in that said tanning agent is prepared according to the following process: mixing lignosulfonate, absolute ethyl alcohol and ammonia water, performing ultrasonic dispersion, dropwise adding tetraethyl silicate at 50-65 ℃, stirring for 8-12 hours at 50-65 ℃, performing centrifugal separation, and collecting a filter cake; mixing the filter cake with polyaspartic acid and deionized water, stirring for 20-22 h at the pH of 3.5-4.5 and the temperature of 60-70 ℃, performing centrifugal separation again, mixing the separated solid with acrylic resin, performing ultrasonic dispersion, and stirring for 2-3 h to obtain the product.
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| CN112176128B (en) * | 2020-10-30 | 2021-11-30 | 陕西科技大学 | Method for synthesizing ZnZr-MOF-LDH nano tanning agent based on template-oriented method |
| CN113278744B (en) * | 2021-06-05 | 2022-04-01 | 百草边大生物科技(青岛)有限公司 | Preparation method of cow leather containing bioactive components |
| CN114410855B (en) * | 2022-02-24 | 2022-10-11 | 四川大学 | Chromium-free tanning process for ecological leather |
| FR3142200A1 (en) * | 2022-11-22 | 2024-05-24 | Ctc | Process for preparing leather comprising the use of a silylated compound and leather obtained by this process |
| CN115772586B (en) * | 2022-12-08 | 2024-04-09 | 百草边大生物科技(青岛)有限公司 | Preparation method of antibacterial and peculiar smell removing cow leather containing pinus massoniana needle and cedarwood extracts |
| CN117683951B (en) * | 2024-01-23 | 2024-08-23 | 步威（清远）皮革有限公司 | High-strength tear-resistant cattle two-layer counter-fur and preparation process thereof |
| CN117683950B (en) * | 2024-01-23 | 2024-08-23 | 步威（清远）皮革有限公司 | Cattle counter-fur capable of being directly adhered without sewing and preparation process thereof |
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| CN102134619A (en) * | 2011-02-25 | 2011-07-27 | 上海百宜装饰工程设计有限公司 | Buffalo hide leather treating method |
| CN105132596A (en) * | 2015-07-30 | 2015-12-09 | 兴业皮革科技股份有限公司 | Production technology of cow skin nappa leather |
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| CN101240354A (en) * | 2008-03-12 | 2008-08-13 | 河南大学 | Acrylic resin/SiO2 nano composite tanning agent and preparation method thereof |
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