CN109609707B

CN109609707B - Preparation method of reflective leather

Info

Publication number: CN109609707B
Application number: CN201910101088.9A
Authority: CN
Inventors: 雷丙南; 许燕杰; 林汉彬; 许维奇; 陈启明
Original assignee: Zhangzhou Xiangzhou Leather Co ltd
Current assignee: Zhangzhou Xiangzhou Leather Co ltd
Priority date: 2019-01-31
Filing date: 2019-01-31
Publication date: 2021-07-20
Anticipated expiration: 2039-01-31
Also published as: CN109609707A

Abstract

The invention discloses a preparation method of reflective leather, and belongs to the technical field of leather. The preparation method of the reflective leather comprises the following steps: putting the leather blank into a rotary drum, and obtaining the reflective leather after water returning, retanning and down extracting, neutralizing, pre-adding ester, dyeing, adding ester, fixing color, product surface treatment and secondary treatment in sequence, wherein the secondary treatment comprises the following steps: secondary water return, secondary ester addition, secondary dyeing, secondary color fixation, drying and softening. The reflective leather prepared by the invention has strong velvet feeling and high softness.

Description

Preparation method of reflective leather

Technical Field

The invention belongs to the technical field of leather, and particularly relates to a preparation method of reflective leather.

Background

With the development of society, the living standard of people is higher and higher, and the personal belongings are required to have high quality and certain aesthetic feeling. Leather products are popular among people because of their advantages of high durability and long service life. However, the traditional leather products are pursuing the strength, the texture characteristics and the waterproof performance, and few innovations are made on other performances of the leather products, so that one leather product can not attract consumers at a time.

Therefore, it is required to provide a reflective leather having a strong nap feeling and high softness.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide the reflective leather with strong velvet feeling and high softness.

The invention adopts the following technical scheme:

the preparation method of the reflective leather comprises the following steps:

putting the leather blank into a rotary drum, and obtaining the reflective leather after water returning, retanning and down extracting, neutralizing, pre-adding ester, dyeing, adding ester, fixing color, product surface treatment and secondary treatment in sequence, wherein the secondary treatment comprises the following steps: secondary water return, secondary ester addition, secondary dyeing, secondary color fixation, drying and softening;

the pre-esterification process is concretely as follows: according to the mass percentage of the leather blank, 1-3% of EG60 and 1-4% of dodecyl phosphate monoester are put into a rotary drum, and the rotary drum runs for 30-40 min;

the dyeing process is specifically as follows: according to the mass percentage of the leather blank, 2-4% of UR, 2-4% of dispersing agent, 1-3% of XAR and 1-3% of ammonia water are put into a rotary drum, then dye is added into the rotary drum, and the rotary drum runs for 60-70 min.

Further, the water return process is specifically as follows: according to the mass percentage of the leather blank, 200-230% of water with the temperature of 40-50 ℃, 0.4-0.6% of OC and 0.5-0.7% of moisture regaining agent are put into a rotary drum, after the rotary drum runs for 60-70 min, 1-3% of ammonium sulfate is put into the rotary drum, after the rotary drum runs for 90-100 min, 0.7-1.0% of phosphoglyceride, 0.1-0.4% of polyethylene oxide, 1-3% of softening enzyme, 0.6-0.8% of oxalic acid and 0.4-0.7% of formic acid are put into the rotary drum in the rotary drum and run for 60-70 min, liquid in the rotary drum is discharged, and then water is added for washing for 5-10 min, and then water is discharged.

Further, the retanning and wool extracting process comprises the following steps of putting 100-110% of water and 0.3-0.5% of formic acid into a rotary drum according to the mass percentage of the leather blank, after the rotary drum runs for 30-40 min, the pH value of liquid in the rotary drum is 2.8-3.2, then putting 1.5-2.0% of FM120 into the rotary drum, after the rotary drum runs for 30-40 min, putting 4-6% of chromium powder into the rotary drum, after the rotary drum runs for 90-100 min, putting 80-90% of water and 1-3% of sodium formate into the rotary drum, after the rotary drum runs for 30-40 min, putting 0.5-0.7% of baking soda again, after the rotary drum runs for 30-40 min, the pH value of liquid in the rotary drum is 4.0-4.5, then discharging the liquid in the rotary drum, adding water, and washing for 10-5 min, and then discharging water.

Further, the neutralization process specifically comprises the following steps: according to the mass percentage of the leather blank, 120-130% of water, 2-3% of sodium formate and 2-3% of NA are put into a rotary drum, after the rotary drum runs for 40-50 min, 1-3% of sodium bicarbonate, 0.5-0.7% of sodium sulfite and 1-3% of sodium bicarbonate are put into the rotary drum, after the rotary drum runs for 120-130 min, the pH value of liquid in the rotary drum is 5.8-6.0, then the liquid in the rotary drum is discharged, water is added for washing for 5-10 min, and then the water is discharged.

Further, the color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 100-110% of water with the temperature of 40-50 ℃ is added into a rotary drum, after the rotary drum runs for 5-10 min, formic acid is added into the rotary drum, the amount of 0.5-0.8% is added each time, and the running time of the rotary drum is 10-15 min, 10-15 min and 15-20 min in sequence each time, then the water in the rotary drum is discharged, water is added for washing, then the water is discharged, and the leather blank after color fixing treatment is taken out.

Further, the surface treatment of the product comprises the steps of pasting, drying, softening and buffing, wherein the temperature during drying is 65-75 ℃, the humidity is 10-12%, and the buffing is carried out by using No. 180 coarse sand paper.

Further, in the secondary treatment process, the secondary water return process specifically includes: according to the mass percentage of the leather blank, 300-320% of water and 0.8-1.2% of sodium formate are put into a rotary drum, the rotary drum operates for 25-30 min, then liquid in the rotary drum is discharged, and then water is added for washing for 5-10 min and then the water is discharged.

Further, the ester adding process is specifically as follows: according to the mass percentage of the leather blank, 50-60% of water with the temperature of 50-55 ℃ is put into a rotary drum, after the rotary drum runs for 50-60 min, 3-5 EG60, 2-3% of AC, 1-2% of YY707, 0.3-0.6% of AK and 0.1-0.3% of mildew preventive are put into the rotary drum, and the rotary drum runs for 55-65 min;

the secondary ester addition process is as follows: according to the mass percentage of the leather blank, 120-130% of water with the temperature of 45-50 ℃, 2-5% of AC, 2-5% of YY707, 0.8-1.2% of AK and 0.1-0.3% of mildew preventive are put into a rotary drum, and the rotary drum runs for 40-50 min.

Further, the secondary dyeing process specifically comprises the following steps: and (3) adding the dye into the rotary drum, and operating the rotary drum for 20-30 min.

Further, the secondary color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 200-220% of water is put into a rotary drum, 0.5-0.8% of formic acid is added into the rotary drum after the rotary drum runs for 20-30 min, 0.7-1.1% of formic acid is added into the rotary drum after the rotary drum runs for 10-15 min, liquid in the rotary drum is discharged after the rotary drum runs for 15-20 min, then 150-170% of water and 1.5-2.0% of AS are added, the liquid in the rotary drum is discharged after the rotary drum runs for 20-30 min, then the leather blank in the rotary drum is taken out, and then a dryer is used for softening.

Compared with the prior art, the invention has the following beneficial effects:

according to the preparation method of the reflective leather, in the water return process, softening enzyme and oxalic acid are used together to soften the leather blank fiber, and polyoxyethylene serving as an emulsifier and a dispersing agent is used to disperse the raw materials in the water return process, so that the raw materials fully react with the leather blank fiber, and impurities on the surface of the leather blank are effectively removed;

secondly, in the retanning process, the FM is adopted to improve the hand feeling of the leather blank and the line-falling uniformity of the leather blank in the process of falling and softening, and meanwhile, the adopted retanning agent FM120 can effectively prevent the surface of the leather blank from being changed and improve the compactness of the leather blank;

thirdly, EG60 with excellent light resistance and dodecyl phosphate monoester with excellent antistatic property are added and mixed for use in the pre-esterification process, and meanwhile, EG60 also has strong permeability and can be matched with the subsequent dyeing process to improve the permeability of dye on the blank fiber, so that the color fastness is effectively improved and the color and luster degree of the blank fiber can be improved;

and fourthly, in the preparation method, secondary ester adding, secondary dyeing and secondary color fixing treatment are adopted, wherein in the secondary ester adding process, the permeability of the grease on the leather blank fiber can be improved by using anionic grease AC and YY707 with strong permeability, the permeability of AK and a mildew inhibitor is driven, and the softness of AK can be improved while the compactness of the grain surface of the leather blank is not influenced, so that the glossiness of the leather product is improved, and the leather product has a strong light reflecting effect.

Detailed Description

The raw materials adopted by the invention are all commercial products, wherein;

UR is Pasdan UR from Pasteur (China) Co., Ltd; (ii) a

The dispersant is Tamu M from Basff (China) Co.Ltd;

XAR is Pasteur XAR from Pasteur (China) Ltd;

707 is SYNTHOL YY707 available from Schmidt (Nanjing) leather chemicals, Inc.;

AK is POLYOL AK available from Schmidt (Nanjing) leather chemicals, Inc.;

the mildew preventive is a mildew preventive TJ-A2233 purchased from New materials GmbH, Sichuan;

AC is SYNTHOL AC available from Schmidt (Nanjing) leather chemicals, Inc.;

FM is SYNTHOL FM120 available from Schmidt (Nanjing) leather chemicals, Inc.;

NA is Tam NA from Pasteur, Inc. of Bassfer (China);

EG60 is sulpirol EG60 available from smith (nanjing) leather chemicals, inc;

the softening enzyme is TRUPOZYM CL of Toepler chemical dye (Jiaxing) Co., Ltd;

OC is Youshanbang OC from Pasteur (China) Ltd;

the rewetting agent is Youshaban W available from BASF (China) Inc.;

AS is Bardanan AS from Pasteur (China) Ltd.

Example 1

The preparation method of the reflective leather comprises the following steps:

putting the leather blank into a rotary drum, and obtaining the reflective leather after water returning, retanning and down extracting, neutralizing, pre-esterification, dyeing, ester adding and color fixing, product surface treatment and secondary treatment in sequence, wherein the secondary treatment comprises the following steps: secondary water return, secondary ester addition, secondary dyeing, secondary color fixation, drying and softening.

The water return process is as follows: according to the mass percentage of the leather blank, 200% of water with the temperature of 40 ℃, 0.4% of OC and 0.5% of moisture regaining agent are put into a rotary drum, after the rotary drum runs for 60min, 1% of ammonium sulfate is put into the rotary drum, after the rotary drum runs for 90min, 0.7% of phosphoglyceride, 0.1% of polyethylene oxide, 1% of softening enzyme, 0.6% of oxalic acid and 0.4% of formic acid are put into the rotary drum in the rotary drum and run for 60min, liquid in the rotary drum is discharged, then water is added for washing for 5min, and then water is discharged.

The retanning and wool extracting process is specifically as follows, according to the leather blank, 100% of water and 0.3% of formic acid are put into a rotary drum, after the rotary drum runs for 30min, the pH value of liquid in the rotary drum is 2.8, then 1.5% of FM120 rotary drum is put into the rotary drum, after the rotary drum runs for 30min, 4% of chromium powder is put into the rotary drum, after the rotary drum runs for 90min, 80% of water and 1% of sodium formate are put into the rotary drum, after the rotary drum runs for 30min, 0.5% of baking soda is put into the rotary drum again, after the rotary drum runs for 30min, the pH value of liquid in the rotary drum is 4.0, then the liquid in the rotary drum is discharged, then water is added for washing for 5min, and then the water is discharged.

The neutralization process is specifically as follows: according to the mass percentage of the leather blank, 120% of water, 2% of sodium formate and 2% of NA are put into a rotary drum, after the rotary drum runs for 40min, 1% of sodium bicarbonate, 0.5% of sodium sulfite and 1% of sodium bicarbonate are put into the rotary drum, after the rotary drum runs for 120min, the pH value of liquid in the rotary drum is 5.8, then the liquid in the rotary drum is discharged, water is added for washing for 5min, and then the water is discharged.

The pre-esterification process is concretely as follows: according to the weight percentage of the leather blank, 1 percent of EG60 and 1 percent of dodecyl phosphate monoester are put into a rotary drum, and the rotary drum runs for 30 min.

The dyeing process is specifically as follows: according to the mass percentage of the leather blank, 2% of UR, 2% of dispersant, 1% of XAR and 1% of ammonia water are put into a rotary drum, then the dye is added into the rotary drum, and the rotary drum runs for 60 min.

The ester addition process is specifically as follows: according to the mass percentage of the leather blank, 50 percent of water with the temperature of 50 ℃ is put into a rotary drum, after the rotary drum runs for 50min, 3EG60, 2 percent of AC, 1 percent of YY707, 0.3 percent of AK and 0.1 percent of mildew preventive are put into the rotary drum, and the rotary drum runs for 55 min.

The color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 100% of water with the temperature of 40 ℃ is added into a rotary drum, after the rotary drum runs for 5min, formic acid is added into the rotary drum, the amount of the formic acid is 0.5% each time, and the running time of the rotary drum is 10min, 10min and 15min in sequence each time, then the water in the rotary drum is discharged, water is added for washing, then the water is discharged, and the leather blank after color fixing treatment is taken out.

The product surface treatment comprises plate pasting, drying, softening and buffing, wherein the temperature during drying is 65 ℃, the dryness and humidity are 10%, and the buffing is carried out by using No. 180 coarse sand paper.

In the secondary treatment process, the secondary water return process is specifically as follows: according to the mass percentage of the leather blank, 300 percent of water and 0.8 percent of sodium formate are put into a rotary drum, the liquid in the rotary drum is discharged after the rotary drum runs for 25min, and then the water is discharged after the water is added for washing for 5 min.

The secondary ester addition process is as follows: according to the mass percentage of the leather blank, 120 percent of water with the temperature of 45 ℃, 2 percent of AC, 2 percent of YY707, 0.8 percent of AK and 0.1 percent of mildew preventive are put into a rotary drum, and the rotary drum runs for 40 min.

The secondary dyeing process is as follows: the dye was added to the drum and the drum was run for 20 min.

The secondary color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 200% of water is put into a rotary drum, 0.5% of formic acid is added into the rotary drum after the rotary drum runs for 20min, 0.7% of formic acid is added into the rotary drum after the rotary drum runs for 10min, liquid in the rotary drum is discharged after the rotary drum runs for 15min, then 150% of water and 1.5% of AS are added, the liquid in the rotary drum is discharged after the rotary drum runs for 20min, then the leather blank in the rotary drum is taken out, and then a dryer is used for softening.

Example 2

The preparation method of the reflective leather comprises the following steps:

The water return process is as follows: according to the mass percentage of the leather blank, 210% of 42 ℃ water, 0.5% of OC and 0.6% of moisture regaining agent are put into a rotary drum, 2% of ammonium sulfate is put into the rotary drum after the rotary drum runs for 62min, 0.8% of phosphoglyceride, 0.2% of polyethylene oxide, 2% of softening enzyme, 0.7% of oxalic acid and 0.5% of formic acid are put into the rotary drum in the rotary drum and run for 62min, liquid in the rotary drum is discharged, then water is added for washing for 6min, and then water is discharged.

The retanning and wool extracting process is specifically as follows, according to the leather blank, 102% of water and 0.4% of formic acid are put into a rotary drum, after the rotary drum runs for 32min, the pH value of liquid in the rotary drum is 2.9, then 1.6% of FM120 rotary drum is put into the rotary drum, after the rotary drum runs for 32min, 5% of chromium powder is put into the rotary drum, after the rotary drum runs for 92min, 82% of water and 2% of sodium formate are put into the rotary drum, after the rotary drum runs for 32min, 0.6% of baking soda is put into the rotary drum again, after the rotary drum runs for 32min, the pH value of liquid in the rotary drum is 4.2, then the liquid in the rotary drum is discharged, then water is added for washing for 6min, and then the water is discharged.

The neutralization process is specifically as follows: according to the mass percentage of the leather blank, 122% of water, 3% of sodium formate and 3% of NA are put into a rotary drum, 2% of sodium bicarbonate, 0.6% of sodium sulfite and 2% of sodium bicarbonate are put into the rotary drum after the rotary drum runs for 42min, the pH value of liquid in the rotary drum is 5.9 after the rotary drum runs for 122min, then the liquid in the rotary drum is discharged, water is added for washing for 6min, and then the water is discharged.

The pre-esterification process is concretely as follows: according to the weight percentage of the blank, 2 percent of EG60 and 2 percent of dodecyl phosphate monoester are put into a rotary drum, and the rotary drum runs for 32 min.

The dyeing process is specifically as follows: according to the mass percentage of the leather blank, 3% of UR, 3% of dispersant, 2% of XAR and 2% of ammonia water are put into a rotary drum, then dye is added into the rotary drum, and the rotary drum runs for 62 min.

The ester addition process is specifically as follows: according to the mass percentage of the leather blank, 52 percent of water with the temperature of 52 ℃ is put into a rotary drum, after the rotary drum runs for 52min, 4EG60, 3 percent of AC, 2 percent of YY707, 0.4 percent of AK and 0.2 percent of mildew preventive are put into the rotary drum, and the rotary drum runs for 58 min.

The color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 102% of water with the temperature of 42 ℃ is added into a rotary drum, after the rotary drum runs for 6min, formic acid is added into the rotary drum, the amount of the formic acid is 0.6% each time, and the running time of the rotary drum is 12min, 12min and 16min in sequence each time, then the water in the rotary drum is discharged, water is added for washing, then the water is discharged, and the leather blank after color fixing treatment is taken out.

The product surface treatment comprises plate pasting, drying, softening and buffing, wherein the temperature during drying is 68 ℃, the dryness and humidity are 11%, and the buffing is carried out by using No. 180 coarse sand paper.

In the secondary treatment process, the secondary water return process is specifically as follows: according to the mass percentage of the leather blank, 305 percent of water and 0.9 percent of sodium formate are put into a rotary drum, the liquid in the rotary drum is discharged after the rotary drum runs for 26min, and then the water is discharged after the water is added for washing for 6 min.

The secondary ester addition process is as follows: according to the mass percentage of the blank, 122 percent of water with the temperature of 46 ℃, 3 percent of AC, 3 percent of YY707, 0.9 percent of AK and 0.2 percent of mildew preventive are put into a rotary drum, and the rotary drum runs for 42 min.

The secondary dyeing process is as follows: the dye was added to the drum and the drum was run for 22 min.

The secondary color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 205% of water is put into a rotary drum, 0.6% of formic acid is added into the rotary drum after the rotary drum runs for 22min, 0.8% of formic acid is added into the rotary drum after the rotary drum runs for 12min, liquid in the rotary drum is discharged after the rotary drum runs for 16min, then 155% of water and 1.6% of AS are added, the liquid in the rotary drum is discharged after the rotary drum runs for 22min, then the leather blank in the rotary drum is taken out, and then a dryer is used for softening.

Example 3

The preparation method of the reflective leather comprises the following steps:

The water return process is as follows: according to the mass percentage of the leather blank, 220% of 48 ℃ water, 0.6% of OC and 0.7% of moisture regaining agent are put into a rotary drum, 2% of ammonium sulfate is put into the rotary drum after the rotary drum runs for 68min, 0.9% of phosphoglyceride, 0.3% of polyethylene oxide, 3% of softening enzyme, 0.8% of oxalic acid and 0.6% of formic acid are put into the rotary drum in the rotary drum after the rotary drum runs for 98min, liquid in the rotary drum is discharged, then water is added for washing for 9min, and then water is discharged.

The retanning and wool extracting process is specifically as follows, according to the leather blank, 108% of water and 0.5% of formic acid are put into a rotary drum, after the rotary drum runs for 38min, the pH value of liquid in the rotary drum is 3.1, then 1.8% of FM120 is put into the rotary drum, after the rotary drum runs for 38min, 6% of chromium powder is put into the rotary drum, after the rotary drum runs for 98min, 88% of water and 3% of sodium formate are put into the rotary drum, after the rotary drum runs for 38min, 0.7% of baking soda is put into the rotary drum again, after the rotary drum runs for 38min, the pH value of liquid in the rotary drum is 4.4, then the liquid in the rotary drum is discharged, then water is added for washing for 8min, and then the water is discharged.

The neutralization process is specifically as follows: according to the mass percentage of the leather blank, 128% of water, 3% of sodium formate and 3% of NA are put into a rotary drum, after the rotary drum runs for 48min, 3% of sodium bicarbonate, 0.7% of sodium sulfite and 3% of sodium bicarbonate are put into the rotary drum, after the rotary drum runs for 128min, the pH value of liquid in the rotary drum is 6.1, then the liquid in the rotary drum is discharged, water is added for washing for 8min, and then the water is discharged.

The pre-esterification process is concretely as follows: according to the mass percentage of the blank, 3% of EG60 and 3% of dodecyl phosphate monoester are put into a rotary drum, and the rotary drum runs for 30-40 min.

The dyeing process is specifically as follows: according to the mass percentage of the leather blank, 4% of UR, 3% of dispersant, 3% of XAR and 3% of ammonia water are put into a rotary drum, then the dye is added into the rotary drum, and the rotary drum runs for 68 min.

The ester addition process is specifically as follows: according to the mass percentage of the leather blank, 58 percent of water with the temperature of 54 ℃ is put into a rotary drum, 5EG60, 3 percent of AC, 2 percent of YY707, 0.5 percent of AK and 0.3 percent of mildew preventive are put into the rotary drum after the rotary drum runs for 58min, and the rotary drum runs for 62 min.

The color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 108% of 48 ℃ water is added into a rotary drum, after the rotary drum runs for 8min, formic acid is added into the rotary drum, the amount of the formic acid is 0.7% each time, and the running time of the rotary drum is 14min, 14min and 18min in sequence each time, then the water in the rotary drum is discharged, water is added for washing, then the water is discharged, and the leather blank after color fixing treatment is taken out.

The product surface treatment comprises plate pasting, drying, softening and buffing, wherein the temperature during drying is 72 ℃, the dryness and humidity are 12%, and the buffing is carried out by using No. 180 coarse sand paper.

In the secondary treatment process, the secondary water return process is specifically as follows: according to the mass percentage of the leather blank, 315 percent of water and 1.1 percent of sodium formate are put into a rotary drum, the liquid in the rotary drum is discharged after the rotary drum runs for 28min, and then the water is discharged after the rotary drum is washed by adding water for 8 min.

The secondary ester addition process is as follows: according to the mass percentage of the leather blank, 128% of 48 ℃ water, 4% of AC, 4% of YY707, 1.1% of AK and 0.3% of mildew preventive are put into a rotary drum, and the rotary drum runs for 48 min.

The secondary dyeing process is as follows: the dye was added to the drum and the drum was run for 28 min.

The secondary color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 215% of water is put into a rotary drum, 0.7% of formic acid is added into the rotary drum after the rotary drum runs for 28min, 1.0% of formic acid is added into the rotary drum after the rotary drum runs for 14min, liquid in the rotary drum is discharged after the rotary drum runs for 18min, then 165% of water and 1.8% of AS are added, the liquid in the rotary drum is discharged after the rotary drum runs for 28min, then the leather blank in the rotary drum is taken out, and then a dryer is used for softening.

Example 4

The preparation method of the reflective leather comprises the following steps:

The water return process is as follows: according to the mass percentage of the leather blank, 230 percent of water with the temperature of 50 ℃, 0.6 percent of OC and 0.7 percent of moisture regaining agent are put into a rotary drum, after the rotary drum runs for 70min, 3 percent of ammonium sulfate is put into the rotary drum, after the rotary drum runs for 100min, 1.0 percent of phosphoglyceride, 0.4 percent of polyoxyethylene, 3 percent of softening enzyme, 0.8 percent of oxalic acid and 0.7 percent of formic acid are put into the rotary drum in the rotary drum and run for 70min, the liquid in the rotary drum is discharged, then water is added for washing for 10min, and then water is discharged.

The retanning and wool extracting process is specifically as follows, according to the leather blank, according to the mass percentage, 110% of water and 0.5% of formic acid are put into a rotary drum, after the rotary drum runs for 40min, the pH value of liquid in the rotary drum is 3.2, then 2.0% of FM120 is put into the rotary drum, after the rotary drum runs for 40min, 6% of chromium powder is put into the rotary drum, after the rotary drum runs for 100min, 90% of water and 3% of sodium formate are put into the rotary drum, after the rotary drum runs for 40min, 0.7% of baking soda is put into the rotary drum again, after the rotary drum runs for 40min, the pH value of liquid in the rotary drum is 4.5, then the liquid in the rotary drum is discharged, then water is added for washing for 10min, and then the water is discharged.

The neutralization process is specifically as follows: according to the mass percentage of the leather blank, 130% of water, 3% of sodium formate and 3% of NA are put into a rotary drum, after the rotary drum runs for 50min, 3% of sodium bicarbonate, 0.7% of sodium sulfite and 3% of sodium bicarbonate are put into the rotary drum, after the rotary drum runs for 130min, the pH value of liquid in the rotary drum is 6.0, then the liquid in the rotary drum is discharged, water is added for washing for 10min, and then the water is discharged.

The pre-esterification process is concretely as follows: according to the weight percentage of the leather blank, 3 percent of EG60 and 4 percent of dodecyl phosphate monoester are put into a rotary drum, and the rotary drum runs for 40 min.

The dyeing process is specifically as follows: according to the mass percentage of the leather blank, 4% of UR, 4% of dispersant, 3% of XAR and 3% of ammonia water are put into a rotary drum, then dye is added into the rotary drum, and the rotary drum runs for 70 min.

The ester addition process is specifically as follows: according to the mass percentage of the leather blank, 60 percent of water with the temperature of 55 ℃ is put into a rotary drum, after the rotary drum runs for 60min, 5 percent of EG60, 3 percent of AC, 2 percent of YY707, 0.6 percent of AK and 0.3 percent of mildew preventive are put into the rotary drum, and the rotary drum runs for 65 min.

The color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 110% of water with the temperature of 50 ℃ is added into a rotary drum, after the rotary drum runs for 10min, formic acid is added into the rotary drum, the amount of the formic acid is 0.8% each time, and the running time of the rotary drum is 15min, 15min and 20min in sequence each time, then the water in the rotary drum is discharged, water is added for washing, then the water is discharged, and the leather blank after color fixing treatment is taken out.

The product surface treatment comprises plate pasting, drying, softening and buffing, wherein the temperature during drying is 75 ℃, the dryness and humidity are 12%, and the buffing is carried out by using No. 180 coarse sand paper.

In the secondary treatment process, the secondary water return process is specifically as follows: according to the mass percentage of the leather blank, 320 percent of water and 1.2 percent of sodium formate are put into a rotary drum, the liquid in the rotary drum is discharged after the rotary drum runs for 30min, and then the water is discharged after the water is added for washing for 10 min.

The secondary ester addition process is as follows: according to the mass percentage of the leather blank, 130 percent of water with the temperature of 50 ℃, 5 percent of AC, 5 percent of YY707, 1.2 percent of AK and 0.3 percent of mildew preventive are put into a rotary drum, and the rotary drum runs for 50 min.

The secondary dyeing process is as follows: the dye was added to the drum and the drum was run for 30 min.

The secondary color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 220% of water is put into a rotary drum, 0.8% of formic acid is added into the rotary drum after the rotary drum runs for 30min, 1.1% of formic acid is added into the rotary drum after the rotary drum runs for 15min, liquid in the rotary drum is discharged after the rotary drum runs for 20min, then 170% of water and 2.0% of AS are added, the liquid in the rotary drum is discharged after the rotary drum runs for 30min, then the leather blank in the rotary drum is taken out, and then a dryer is used for softening.

Comparative example 1

The preparation method of the reflective leather comprises the following steps:

The water return process is as follows: according to the mass percentage of the leather blank, 230 percent of 50 ℃ water, 0.6 percent of OC and 0.7 percent of moisture regaining agent are put into a rotary drum, after the rotary drum runs for 70min, 3 percent of ammonium sulfate is put into the rotary drum, after the rotary drum runs for 100min, 3 percent of softening enzyme, 0.8 percent of oxalic acid and 0.7 percent of formic acid are put into the rotary drum and run for 70min, the liquid in the rotary drum is discharged, then water is added for washing for 10min, and then water is discharged.

Comparative example 2

The preparation method of the reflective leather comprises the following steps:

The ester addition process is specifically as follows: according to the mass percentage of the leather blank, 60 percent of water with the temperature of 55 ℃ is put into a rotary drum, after the rotary drum runs for 60min, 5EG60, 3 percent of AC, 2 percent of YY707, 0.6 percent of AK and 0.3 percent of mildew preventive are put into the rotary drum, and the rotary drum runs for 65 min.

The product surface treatment comprises plate pasting, drying, softening and buffing, wherein the temperature during drying is 75 ℃, the dryness and humidity are 12%, the buffing is treated by 180-size coarse abrasive paper, and then the leather blank is taken out to be softened by a dryer, so that the reflective leather is obtained.

The reflective leather prepared in the embodiments 1 to 4 and the comparative examples 1 to 2 of the present invention was tested, wherein:

firstly, detecting the water splashing prevention performance:

carrying out a water-splashing prevention test by using a water-wetting degree tester GT-7033N;

note that:

1.1 and 250mL of water must be sprayed within 25-30 s;

1.2, forming an angle of 45 degrees on a horizontal plane by the sample bracket;

1.3, keeping a distance of 152.4mm between the center of the lower surface of the nozzle and the center of the surface of the sample;

1.4, during the test, the hand is prevented from being released from the detection instrument, so that the experimental result is not influenced.

Secondly, a softness testing method comprises the following steps:

sampling according to the sampling mode of ISO 2418-;

thirdly, testing color fastness:

color fastness test was performed by using a manual crocking decolorant GT-7034-B manufactured by Goodywell detection instruments (Qingdao) Co., Ltd.;

fourthly, testing the abrasion performance:

the leather abrasion test is carried out by an universal abrasion tester GT-7012-S manufactured by Shenzhen Yinfei electronic technology Limited;

fifthly, tension testing:

the tensile test was conducted by a tensile tester GT-7010-EP sold by Shandong Ziquan Instrument sales center.

Sixthly, testing yellowing resistance:

and (4) carrying out a yellowing resistance test by a yellowing resistance tester.

The reflective leather obtained in the embodiments 1 to 3 of the present invention was tested by a tensile testing machine, a yellowing resistance testing machine and a universal abrasion testing machine, and the test results are shown in table 1 below;

table 1: the detection results of the reflective leather of examples 1 to 4 and comparative examples 1 to 1 were as follows:

as can be seen from Table 1, the reflective leather prepared by the preparation method of the invention has strong tearing strength reaching 173N in the transverse direction and 153N in the longitudinal direction, tensile strength reaching 39N in the transverse direction and 28N in the longitudinal direction, dynamic water resistance reaching 3000+ times, and water-staining degree reaching 80. The tearing strength of the comparative example is 130N in the transverse direction and 121N in the longitudinal direction, the tensile strength is 21N in the transverse direction and 23N in the longitudinal direction, the dynamic waterproof performance is 2500+ times, the water degree is 70, and the performance is obviously lower than that of the examples 1-4.

While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims

1. The preparation method of the reflective leather is characterized by comprising the following steps:

putting the leather blank into a rotary drum, and obtaining the reflective leather after water returning, retanning and down extracting, neutralizing, pre-fatliquoring, dyeing, fatliquoring, color fixing, product surface treatment and secondary treatment in sequence, wherein the secondary treatment comprises the following steps: secondary water return, secondary fat adding, secondary dyeing, secondary color fixing, drying and softening;

the pre-fatliquoring process is as follows: according to the mass percentage of the leather blank, 1-3% of EG60 and 1-4% of dodecyl phosphate monoester are put into a rotary drum, and the rotary drum runs for 30-40 min;

the dyeing process is specifically as follows: according to the mass percentage of the leather blank, 2-4% of UR, 2-4% of dispersing agent, 1-3% of XAR and 1-3% of ammonia water are put into a rotary drum, then dye is added into the rotary drum, and the rotary drum runs for 60-70 min;

the water return process is as follows: according to the mass percentage of the leather blank, 200-230% of water with the temperature of 40-50 ℃, 0.4-0.6% of OC and 0.5-0.7% of moisture regaining agent are put into a rotary drum, after the rotary drum runs for 60-70 min, 1-3% of ammonium sulfate is put into the rotary drum, after the rotary drum runs for 90-100 min, 0.7-1.0% of phosphoglyceride, 0.1-0.4% of polyethylene oxide, 1-3% of softening enzyme, 0.6-0.8% of oxalic acid and 0.4-0.7% of formic acid are put into the rotary drum in the rotary drum and run for 60-70 min, liquid in the rotary drum is discharged, and then water is added for washing for 5-10 min, and then water is discharged;

the retanning and wool extracting process comprises the following steps of putting 100-110% of water and 0.3-0.5% of formic acid into a rotary drum according to the mass percentage of a leather blank, putting the rotary drum into a drum, after the rotary drum runs for 30-40 min, the pH value of liquid in the drum is 2.8-3.2, then putting 1.5-2.0% of FM120 into the rotary drum, after the rotary drum runs for 30-40 min, putting 4-6% of chromium powder into the rotary drum, after the rotary drum runs for 90-100 min, putting 80-90% of water and 1-3% of sodium formate into the rotary drum, after the rotary drum runs for 30-40 min, putting 0.5-0.7% of baking soda again, after the rotary drum runs for 30-40 min, the pH value of liquid in the rotary drum is 4.0-4.5, then discharging the liquid in the rotary drum, then adding water to wash for 5-10 min, and then discharging water;

the neutralization process is specifically as follows: according to the mass percentage of the leather blank, putting 120-130% of water, 2-3% of sodium formate and 2-3% of NA into a rotary drum, after the rotary drum runs for 40-50 min, putting 1-3% of sodium bicarbonate, 0.5-0.7% of sodium sulfite and 1-3% of sodium bicarbonate into the rotary drum, after the rotary drum runs for 120-130 min, the pH value of liquid in the rotary drum is 5.8-6.0, then discharging the liquid in the rotary drum, adding water for washing for 5-10 min, and then discharging the water;

the color fixing process specifically comprises the following steps: adding 100-110% of water with the temperature of 40-50 ℃ into a rotary drum according to the mass percentage of the leather blank, after the rotary drum runs for 5-10 min, adding formic acid into the rotary drum, wherein the adding amount of the formic acid is 0.5-0.8% each time, and the running time of the rotary drum is 10-15 min, 10-15 min and 15-20 min in sequence each time, then discharging the water in the rotary drum, adding water for washing, then discharging the water, and taking out the leather blank after color fixing treatment;

the product surface treatment comprises plate pasting, drying, softening and buffing, wherein the temperature during drying is 65-75 ℃, the humidity is 10-12%, and the buffing is carried out by using No. 180 coarse sand paper;

in the secondary treatment process, the secondary water return process is specifically as follows: according to the mass percentage of the leather blank, 300-320% of water and 0.8-1.2% of sodium formate are put into a rotary drum, liquid in the rotary drum is discharged after the rotary drum runs for 25-30 min, and then water is added for washing for 5-10 min and then the water is discharged;

the fat liquoring process is as follows: according to the mass percentage of the leather blank, 50-60% of water with the temperature of 50-55 ℃ is put into a rotary drum, after the rotary drum runs for 50-60 min, 3-5% of EG60, 2-3% of AC, 1-2% of YY707, 0.3-0.6% of AK and 0.1-0.3% of mildew preventive are put into the rotary drum, and the rotary drum runs for 55-65 min;

the secondary greasing process is as follows: according to the mass percentage of the leather blank, 120-130% of water with the temperature of 45-50 ℃, 2-5% of AC, 2-5% of YY707, 0.8-1.2% of AK and 0.1-0.3% of mildew preventive are put into a rotary drum, and the rotary drum runs for 40-50 min;

the secondary dyeing process is as follows: adding the dye into a rotary drum, and operating the rotary drum for 20-30 min;

the secondary color fixing process specifically comprises the following steps: according to the mass percentage of the leather blank, 200-220% of water is put into a rotary drum, 0.5-0.8% of formic acid is added into the rotary drum after the rotary drum runs for 20-30 min, 0.7-1.1% of formic acid is added into the rotary drum after the rotary drum runs for 10-15 min, liquid in the rotary drum is discharged after the rotary drum runs for 15-20 min, then 150-170% of water and 1.5-2.0% of AS are added, the liquid in the rotary drum is discharged after the rotary drum runs for 20-30 min, then the leather blank in the rotary drum is taken out, and then a dryer is used for softening.