CN105039607B - A kind of preparation method for preparing Chrome Tanning Liquor with shitosan - Google Patents
A kind of preparation method for preparing Chrome Tanning Liquor with shitosan Download PDFInfo
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- CN105039607B CN105039607B CN201510410574.0A CN201510410574A CN105039607B CN 105039607 B CN105039607 B CN 105039607B CN 201510410574 A CN201510410574 A CN 201510410574A CN 105039607 B CN105039607 B CN 105039607B
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Abstract
The present invention relates to a kind of preparation method for preparing Chrome Tanning Liquor with shitosan.Comprise the following steps：The acid solution that organic acid is configured to 0.03 0.06g/ml；It is 20 35 parts of shitosans the above-mentioned organic acid soln dissolving with 20 35 parts to weigh quality；Be that 100 parts of bichromates are dissolved in the water that quality is 400 600 parts, temperature is 65 85 DEG C by quality, obtain dichromate solution, then acid is added in the container equipped with dichromate solution under agitation；The chitosan solution dissolved with organic acid is added slowly with stirring, keeps reaction to complete, solution checks owse color and basicity, and reaction solution is adjusted in aeruginous, until reaction completes and reach requirement, finally stood and display.When Chrome Tanning Liquor is prepared with shitosan, may replace glucose, reduce use cost.The Chrome Tanning Liquor of gained is limited the good combination properties such as excellent feature, tanning properties, wearability, tensile strength with illiteracy.
Description
（One）Technical field
The invention belongs to leather chemical industry field, and in particular to a kind of preparation method for preparing Chrome Tanning Liquor with shitosan.
（Two）Background technology
Tanning is the qualitative change process for making rawhide be converted into leather, and the chemical material that skin is changed into leather can be referred to as tanning agent,
In leather production, spendable tanning agent has inorganic tanning agent and organic tanning agent etc., the chrome tanning in inorganic tanning agent in numerous tanning agents
Agent with the leather of its tanning performance such as have very strong hydrothermal stability, shelf-stable, soft plentiful, dyeability excellent,
So far still there is the effect that cannot be substituted completely.
The common valence state of chromium has：0th ,+3 ,+6 three kinds, the chromium of wherein only trivalent just has flexibility, and chromium is main in nature
Chrome Tanning Liquor in potassium dichromate or sodium dichromate in the form of Cr VI, used in leather production（Or chromium powder）, generally
Add reducing agent to be formulated in acid condition by bichromate, the sexavalence chromic salts without flexibility is reduced to flexibility
Triacidic base formula chromic salts.
But, produce the raw material-red vanadium of chrome tanning agent（Potassium dichromate, sodium dichromate）Not only reserves are limited on earth.And
And, the trivalent chromium in the chrome wastewater not fully absorbed by skin is easy to be changed into the very strong Cr VI of toxicity under certain condition,
Adverse effect is brought to environment.Therefore, further improve chrome-tanned performance, reduce the consumption of chrome tanning agent, increase leather to chrome tanning
The absorption of agent, the utilization rate for improving chrome tanning agent, reduce the discharge of waste liquid, not only can save limited resource and can mitigate
Pollution to environment, with significant economic benefit and social benefit, significant.
（Three）Content of the invention
The present invention is in order to make up the deficiencies in the prior art, there is provided a kind of preparation method for preparing Chrome Tanning Liquor with shitosan,
The preparation method is simple to operate, raw material is easy to get, and the shitosan of gained reduction Chrome Tanning Liquor can not only replace glucose, and have compared with
The limit good combination properties such as feature, tanning properties excellent, wearability, tensile strength is covered well.
The present invention is achieved through the following technical solutions：
A kind of preparation method for preparing Chrome Tanning Liquor with shitosan, which is characterized in that：Comprise the following steps：
（1）The acid solution that organic acid is configured to 0.03-0.06g/ml；
（2）Weigh quality according to the shitosan of 100% meter and above-mentioned organic with 20-35 parts for 20-35 parts, mass concentration
Acid solution dissolves；
（3）By quality be 100 parts, mass concentration be dissolved in quality for 400-600 parts, temperature according to the bichromate of 100% meter
Spend in the water for 65-85 DEG C, obtain dichromate solution, then add in the container equipped with dichromate solution under agitation
A certain amount of acid；
（4）Under agitation to equipped with being slowly added to be dissolved with organic acid in reaction vessel of the dichromate solution with acid solution
Chitosan solution, keep reaction to complete, solution checks owse color and basicity, and reaction solution is adjusted in aeruginous
Whole, until reaction completes and reach requirement, finally stand and display.
Step（1）In, the organic acid is glacial acetic acid（≥99.5%）, formic acid, lactic acid, preferably glacial acetic acid（≥99.5%）.
Step（2）In, the shitosan is obtained through deacetylation by the chitin that nature is widely present, bag
Include the various derivants of common shitosan and shitosan.
Step（3）In, described bichromate is potassium dichromate or sodium dichromate, and the acid is concentrated sulphuric acid, concentrated nitric acid, dense
At least one in hydrochloric acid, perchloric acid, preferably concentrated sulphuric acid.
When described bichromate is potassium dichromate, in potassium bichromate solution, add（133.3-B）Part mass concentration is pressed
According to the acid of 100% meter, wherein B refers to the basicity of target chrome tanning agent.
When described bichromate is sodium dichromate, in sodium dichromate solution, add（132-B）Part mass concentration according to
The acid of 100% meter, wherein B refer to the basicity of target chrome tanning agent.
Beneficial effects of the present invention：When Chrome Tanning Liquor is prepared with shitosan, may replace glucose, reduce use cost.Gained
Chrome Tanning Liquor limit the good combination properties such as excellent feature, tanning properties, wearability, tensile strength with illiteracy.
（Four）Specific embodiment
Embodiment 1：
（1）By glacial acetic acid（≥99.5%）It is configured to the acetic acid solution of 0.05g/ml.
（2）Weigh quality be 20 parts of mass concentrations according to 100% meter shitosan and the step of with 20 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 400 parts, temperature be according to the potassium dichromate of 100% meter
In 75 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（133.3-
B）Concentrated sulphuric acid of part mass concentration according to 100% meter.
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks owse color and alkali in aeruginouss
Degree, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 2：
（1）By glacial acetic acid（≥99.5%）It is configured to the acetic acid solution of 0.05g/ml.
（2）Weigh quality be 30 parts of mass concentrations according to 100% meter shitosan and the step of with 25 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 500 parts, temperature be according to the potassium dichromate of 100% meter
In 75 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（133.3-
B）Concentrated sulphuric acid of part mass concentration according to 100% meter.
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks owse color and alkali in aeruginouss
Degree, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 3：
（1）By glacial acetic acid（≥99.5%）It is configured to the acetic acid solution of 0.05g/ml.
（2）Weigh quality be 35 parts of mass concentrations according to 100% meter shitosan and the step of with 30 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 600 parts, temperature be according to the potassium dichromate of 100% meter
In 75 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（133.3-
B）Concentrated sulphuric acid of part mass concentration according to 100% meter.
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks owse color and alkali in aeruginouss
Degree, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 4：
（1）By glacial acetic acid（≥99.5%）It is configured to the acetic acid solution of 0.05g/ml.
（2）Weigh quality be 25 parts of mass concentrations according to 100% meter shitosan and the step of with 35 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 400 parts, temperature be according to the sodium dichromate of 100% meter
In 75 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（132-B）
Concentrated sulphuric acid of part mass concentration according to 100% meter.（B is the basicity for preparing Chrome Tanning Liquor requirement）
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks owse color and alkali in aeruginouss
Degree, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 5：
（1）By glacial acetic acid（≥99.5%）It is configured to the acetic acid solution of 0.05g/ml.
（2）Weigh quality be 30 parts of mass concentrations according to 100% meter shitosan and the step of with 35 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 500 parts, temperature be according to the sodium dichromate of 100% meter
In 75 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（132-B）
Concentrated sulphuric acid of part mass concentration according to 100% meter.
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks tan in aeruginouss
Liquid color and basicity, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 6：
（1）The formic acid solution that formic acid is configured to 0.05g/ml.
（2）Weigh quality be 35 parts of mass concentrations according to 100% meter shitosan and the step of with 35 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 550 parts, temperature be according to the sodium dichromate of 100% meter
In 75 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（132-B）
Concentrated nitric acid of part mass concentration according to 100% meter.（B is the basicity for preparing Chrome Tanning Liquor requirement）
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, carries out redox reaction, keeps reaction to complete, and solution is in aeruginouss,
Owse color and basicity is checked, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 7：
（1）The lactic acid solution that lactic acid is configured to 0.05g/ml.
（2）Weigh quality be 35 parts of mass concentrations according to 100% meter shitosan and the step of with 25 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 450 parts, temperature be according to the potassium dichromate of 100% meter
In 75 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（133.3-
B）Concentrated hydrochloric acid of part mass concentration according to 100% meter.
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks owse color and alkali in aeruginouss
Degree, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 8：
（1）The lactic acid solution that lactic acid is configured to 0.05g/ml.
（2）Weigh quality be 32 parts of mass concentrations according to 100% meter shitosan and the step of with 30 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 500 parts, temperature be according to the sodium dichromate of 100% meter
In 75 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（132-B）
Perchloric acid of part mass concentration according to 100% meter.
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks owse color and alkali in aeruginouss
Degree, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 9：
（1）By glacial acetic acid（≥99.5%）It is configured to the acetic acid solution of 0.03g/ml.
（2）Weigh quality be 30 parts of mass concentrations according to 100% meter shitosan and the step of with 20 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 480 parts, temperature be according to the potassium dichromate of 100% meter
In 85 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（133.3-
B）Concentrated nitric acid of part mass concentration according to 100% meter.
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks owse color and alkali in aeruginouss
Degree, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
Embodiment 10：
（1）The formic acid solution that formic acid is configured to 0.06g/ml.
（2）Weigh quality be 30 parts of mass concentrations according to 100% meter shitosan and the step of with 30 parts（1）The acid of gained
Solution dissolves.
（3）It is 100 parts of mass concentrations by quality to be dissolved in quality and for 510 parts, temperature be according to the sodium dichromate of 100% meter
In 65 DEG C of water, potassium bichromate solution is obtained, then added in the container equipped with potassium bichromate solution under agitation（132-B）
Concentrated nitric acid, concentrated sulphuric acid of part mass concentration according to 100% meter, concentrated nitric acid is 4 with concentrated sulphuric acid quality:1.
（4）Under agitation to equipped with being slowly added in reaction vessel of the red vanadium solution with acid solution
The chitosan solution dissolved with organic acid, keeps reaction to complete, and solution checks owse color and alkali in aeruginouss
Degree, and reaction solution is adjusted, until reaction is completed and reaches requirement.
（5）Standing is displayed, that is, obtain preparing Chrome Tanning Liquor with shitosan.
（6）It is spray-dried, that is, obtains the chromium powder that is prepared with shitosan.
In the above-described embodiments, the mass concentration is referred to and is undoped according to the potassium dichromate or sodium dichromate of 100% meter
There are the pure potassium dichromate or sodium dichromate of any impurity, the potassium dichromate or sodium dichromate for typically obtaining from nature not to be
Very pure, therefore, when adding, it should be converted into absolutely pure potassium dichromate or sodium dichromate；
The mass concentration refers to pure sulphuric acid, for example, from the matter of the sulphuric acid that has bought on the market according to the sulphuric acid of 100% meter
Amount concentration is 98%, then in the present embodiment, if the sulphuric acid will be added, the addition of the sulphuric acid is：（133.3-B）/
98% or（132-B）/98%；
The addition of the bright sulfur acid（133.3-B）Or（132-B）In B refer to the basicity of target chrome tanning agent；
One embodiment of the present invention is the foregoing is only, is not all of or unique embodiment, this area is common
Any equivalent conversion that technical staff is taken to technical solution of the present invention by reading description of the invention, is the present invention
Claim covered.
Claims (1)
1. a kind of with shitosan prepare Chrome Tanning Liquor preparation method, it is characterised in that：Comprise the following steps：
（1）The acid solution that organic acid is configured to 0.03-0.06g/ml, the organic acid are glacial acetic acid, formic acid, lactic acid；
（2）Weigh quality for 20-35 parts, mass concentration according to 100% meter shitosan or shitosan derivant and use 20-35
The above-mentioned organic acid soln dissolving of part；
（3）By quality be 100 parts, mass concentration is dissolved in quality according to the bichromate of 100% meter and for 400-600 parts, temperature is
In 65-85 DEG C of water, dichromate solution is obtained, then added in the container equipped with dichromate solution under agitation certain
The acid of amount, described bichromate are potassium dichromate or sodium dichromate, and the acid is concentrated sulphuric acid, concentrated nitric acid, concentrated hydrochloric acid, perchloric acid
In at least one,
To in potassium bichromate solution, add（133.3-B）Acid of part mass concentration according to 100% meter, wherein B refer to target chrome tanning
The basicity of agent,
To in sodium dichromate solution, add（132-B）Acid of part mass concentration according to 100% meter, wherein B refer to target chrome tanning agent
Basicity；
（4）The shell that with organic acid dissolved is slowly added to in the reaction vessel equipped with dichromate solution with acid solution under agitation
The solution of the derivant of polysaccharide or shitosan, keeps reaction to complete, and solution checks owse color and basicity in aeruginouss, and right
Reaction solution is adjusted, until reaction completes and reach requirement, finally stands and displays.
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| CN201510410574.0A CN105039607B (en) | 2015-07-14 | 2015-07-14 | A kind of preparation method for preparing Chrome Tanning Liquor with shitosan |
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Families Citing this family (2)
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| WO2019051754A1 (en) * | 2017-09-14 | 2019-03-21 | 南通优元美术图案设计有限公司 | Preparation method for new energy material of chitosan chromate |
| CN109852740B (en) * | 2019-01-21 | 2021-05-04 | 齐鲁工业大学 | Preparation method for preparing chrome tanning agent by using carboxymethyl cellulose |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3960481A (en) * | 1972-09-27 | 1976-06-01 | Thermanil Chemical Company, Incorporated | Process for tanning leather |
| CN104263861A (en) * | 2014-10-10 | 2015-01-07 | 中国科学院城市环境研究所 | Method for preparing chrome tanning agent from chromium-containing wastewater concentrate in electroplating centralized control area |
-
2015
- 2015-07-14 CN CN201510410574.0A patent/CN105039607B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3960481A (en) * | 1972-09-27 | 1976-06-01 | Thermanil Chemical Company, Incorporated | Process for tanning leather |
| CN104263861A (en) * | 2014-10-10 | 2015-01-07 | 中国科学院城市环境研究所 | Method for preparing chrome tanning agent from chromium-containing wastewater concentrate in electroplating centralized control area |
Non-Patent Citations (1)
| Title |
|---|
| 壳聚糖金属络合鞣剂;付崇禄等;《皮革化工》;19930331;第6-8页 * |
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Effective date of registration: 20210930 Address after: 251800 north of Gongye 1st Road, Yangxin Economic Development Zone, Binzhou City, Shandong Province and east of Yuchuan textiles Patentee after: Yangxin Ruifeng Group Co.,Ltd. Address before: 250353 University Road, Changqing District, Ji'nan, Shandong Province, No. 3501 Patentee before: Qilu University of Technology |