CN103451026B - Modified glutaraldehyde tanning agent and preparation method and applications thereof - Google Patents
Modified glutaraldehyde tanning agent and preparation method and applications thereof Download PDFInfo
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Abstract
The invention relates to the field of biochemical engineering, and particularly relates to a modified glutaraldehyde tanning agent and a preparation method and applications thereof. The modified glutaraldehyde tanning agent comprises the following raw materials in part by weight: 100-300 parts of glutaraldehyde, 50-200 parts of ethylene glycol, 100-300 parts of formaldehyde, 1-50 parts of alkaline substances for adjusting pH value and 1-50 parts of acidic substances for adjusting pH value. The invention also provides a preparation method and applications of the modified glutaraldehyde tanning agent, and a glutaraldehyde tanning agent modified by using the method has extremely low free formaldehyde content.
Description
Technical field
The present invention relates to chemical field, in particular to modified glutaraldehyde tanning agent and its production and use.
Background technology
Glutaraldehyde is a kind of two very alkanoics of active aldehyde that contain, and it is to grow up on the basis of dialdehyde-resin tannage, and as a kind of good tanning agent, it is subject to domestic stranger's favor, and is applied in industry very early.Its feature is as follows: speed and the binding capacity of (1) pelt absorption glutaraldehyde are more outstanding; (2) can there is not autohemagglutination in the glutaraldehyde water solution that tanning is used, thereby can not cause grain resinifying and the phenomenon of hardening and becoming fragile; (3) water-fastness, the sweat proof of glutaraldehyde finished leather and alkaline-resisting effect, tanning is better than formaldehyde separately.Although glutaraldehyde possesses lot of advantages, also there is its weak point, such as turned to be yellow by the finished color of glutaraldehyde tanning, occupy this point and just define it in the application in the fields such as light color leather or white leather.Given this, there are a lot of experts in all sorts of ways both at home and abroad glutaraldehyde is carried out to modification, the technology of relevant modified glutaraldehyde is directly to use modified formaldehyde glutaraldehyde, although the method can solve xanthochromia problem, formaldehyde content free in the glutaraldehyde solution after modification and tanning finished product is a lot.
Summary of the invention
The object of the present invention is to provide modified glutaraldehyde tanning agent and its production and use, to solve the above problems.
A kind of modified glutaraldehyde tanning agent is provided in an embodiment of the present invention, comprise: in parts by weight, 100-300 part glutaraldehyde, 50-200 part ethylene glycol, 100-300 part formaldehyde, 1-50 part are for regulating the alkaline matter, 1-50 part of pH value for regulating the acidic substance of pH value.
Preparation method to modified glutaraldehyde tanning agent that should embodiment, comprising:
Respectively glutaraldehyde and ethylene glycol are joined in reactor, be mixed to get the first mixture;
In described reactor, add for regulating the alkaline matter of pH value, regulating pH value is 7-9;
Described inside reactor is warming up to 80-90 ℃, and is incubated in the first setting-up time, obtain the first product;
In described the first product, add formaldehyde, and described for regulating the alkaline matter of pH value to adding in described reactor, and adjusting pH value is 8-10;
Described inside reactor is warming up to 90-100 ℃, and is incubated in the second setting-up time, obtain the second product;
Described inside reactor is cooled to 70-80 ℃, and adds for regulating the acidic substance of pH value in described reactor, regulate pH value to 3-5, and be incubated in the 3rd setting-up time, obtain third product;
Described third product is vacuumized and obtains modified glutaraldehyde tanning agent.
The embodiment of the present invention provides a kind of purposes of modified glutaraldehyde tanning agent, for the pretan of white leather and/or fur, main tanning and/or retanning.
First spent glycol and glutaraldehyde are to react under alkaline condition in pH value; obtain protecting the glutaraldehyde after aldehyde radical; with formaldehyde, it is carried out to modification again; then in pH value, be to carry out deprotection under acidic conditions; finally vacuumize; just obtain novel modified glutaraldehyde, by the glutaraldehyde tanning agent after the method modification, free formaldehyde is few.
Embodiment
Below by specific embodiment, the present invention is described in further detail.
The embodiment of the present invention provides a kind of modified glutaraldehyde tanning agent, comprise: in parts by weight, 100-300 part glutaraldehyde, 50-200 part ethylene glycol, 100-300 part formaldehyde, 1-50 part are for regulating the alkaline matter, 1-50 part of pH value for regulating the acidic substance of pH value.
Preparation method to modified glutaraldehyde tanning agent that should embodiment, comprising:
Respectively glutaraldehyde and ethylene glycol are joined in reactor, be mixed to get the first mixture;
In described reactor, add for regulating the alkaline matter of pH value, regulating pH value is 7-9;
Described inside reactor is warming up to 80-90 ℃, and is incubated in the first setting-up time, obtain the first product;
In described the first product, add formaldehyde, and described for regulating the alkaline matter of pH value to adding in described reactor, and adjusting pH value is 8-10;
Described inside reactor is warming up to 90-100 ℃, and is incubated in the second setting-up time, obtain the second product;
Described inside reactor is cooled to 70-80 ℃, and adds for regulating the acidic substance of pH value in described reactor, regulate pH value to 3-5, and be incubated in the 3rd setting-up time, obtain third product;
Described third product is vacuumized and obtains modified glutaraldehyde tanning agent.
The embodiment of the present invention provides a kind of purposes of modified glutaraldehyde tanning agent, for the pretan of white leather and/or fur, main tanning and/or retanning.
First spent glycol and glutaraldehyde are to react under alkaline condition in pH value; obtain protecting the glutaraldehyde after aldehyde radical; with formaldehyde, it is carried out to modification again; then in pH value, be to carry out deprotection under acidic conditions; finally vacuumize; just obtain novel modified glutaraldehyde, by the glutaraldehyde tanning agent after the method modification, free formaldehyde is few.
Next by some specific embodiments, describe how to prepare this modified glutaraldehyde tanning agent in detail:
Step 101, takes;
Can adopt following scope in certain embodiments, according to parts by weight meter, take 100-300 part glutaraldehyde, 50-200 part ethylene glycol, 100-300 part formaldehyde, 1-50 part for regulating the alkaline matter, 1-50 part of pH value for regulating the acidic substance of pH value.
Or, can adopt following scope in certain embodiments, according to parts by weight meter, take described in the described glutaraldehyde of 110-150 part, the described ethylene glycol of 80-180 part, the described formaldehyde of 110-200 part, 5-20 part described in alkaline matter for regulating pH value, 5-20 part for regulating the acidic substance of pH value.
Wherein for regulate the alkaline matter of pH value comprise following one or more: sodium carbonate, salt of wormwood, sodium hydroxide, triethylamine, thanomin; When regulating the alkaline matter of pH value to comprise sodium hydroxide, the mass percent concentration of sodium hydroxide is 30%.
For the acidic substance that regulate pH value comprise following one or more: hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, phenylformic acid, oxoethanoic acid.
Step 102, joins glutaraldehyde and ethylene glycol in reactor respectively, is mixed to get the first mixture;
Step 103, opens the reflux condensation mode water on reactor top;
By this step, to the condensation of gas producing in following reaction, and be back in reactor.
Can be understood as: the gas backstreaming that the mode by condensing reflux produces while making to obtain the first product in later step and/or the second product and/or third product.
Step 104 adds the alkaline matter that regulates pH value in reactor;
Owing to having there is the first mixture in reactor, then to the inside, add after the alkaline matter that regulates pH value, can regulate pH value to 7-9, glutaraldehyde and ethylene glycol are reacted under alkaline environment.
Step 105, heats up to the product in reactor;
Glutaraldehyde and ethylene glycol react under alkaline environment, obtain protecting the glutaraldehyde (the first product) after aldehyde radical.Be warming up to 80-90 ℃, and be incubated 2-3 hour (the first setting-up time).
Step 106 adds formaldehyde in the first product;
Step 107 adds for regulating the alkaline matter of pH value in reactor;
In step 106, carried out after 2-3 minute, in reactor, added for regulating the alkaline matter of pH value, regulating pH value is 8-10, is adjusted to the modification environment of formaldehyde.
Step 108, is warming up to 90-100 ℃ by inside reactor, insulation;
Formaldehyde improves reaction, at 90-100 ℃, is incubated 2-3 hour (the second setting-up time), obtains the second product.
Step 109, is cooled to 70-80 ℃ by inside reactor, and adds for regulating the acidic substance of pH value in reactor, regulates pH value to 3-5, and is incubated in the 3rd setting-up time, obtains third product;
Soaking time is 2-3 hour (the 3rd setting-up time).
Step 110, vacuumizes and obtains modified glutaraldehyde tanning agent third product.
The condition vacuumizing is 0.8-1.0Mpa, 50-80 ℃, and the modified glutaraldehyde tanning agent obtaining is colourless or micro-yellow viscous fluid.
This modified glutaraldehyde tanning agent is suitable for pretan, main the tanning or retanning such as light color, white leather and fur.
This modified glutaraldehyde tanning agent overcomes formaldehyde content in tanning agent and tanning finished product and exceeds standard, degradation problem under shrinkage temperature reduction and flexibility.Soft, plentiful, pure white flexible by this new modified glutaraldehyde tanning agent tanning finished product, formaldehyde content is few, and shrinkage temperature obviously improves.
Concrete Preparation Example:
Embodiment 1
(1) 160 parts of 120 parts of glutaraldehyde and ethylene glycol are added respectively in reactor, logical reflux condensation mode water, after stirring, adds 20 parts, 30% sodium hydroxide to make its pH value between 7～9, is warming up to 80～90 ℃, insulation reaction 2～3h;
(2) in above-mentioned solution, add 200 parts, formaldehyde, and add 10 parts, 30% sodium hydroxide to make its pH value between 8～10, be warming up to 90～100 ℃, insulation reaction 2～3h;
(3) be cooled to 70～80 ℃, add 10 parts of hydrochloric acid to make its pH value between 3～5, insulation reaction 2～3h;
(4) above-mentioned solution is transferred in pear shape bottle, in 0.8～1.0Mpa, 50～80 ℃ of situations, vacuumized 2h, obtain colourless or micro-yellow viscous fluid and be modified glutaraldehyde tanning agent.
Embodiment 2
(1) 160 parts of 120g glutaraldehyde and ethylene glycol are added respectively in reactor, logical reflux condensation mode water, after stirring, adds 8 parts of triethylamines to make its pH value between 7～9, is warming up to 80～90 ℃, insulation reaction 2～3h;
(2) in above-mentioned solution, add 200 parts, formaldehyde, and add 5 parts of triethylamines to make its pH value between 8～10, be warming up to 90～100 ℃, insulation reaction 2～3h;
(3) be cooled to 70～80 ℃, add 5 parts of sulfuric acid to make its pH value between 3～5, insulation reaction 2～3h;
(4) above-mentioned solution is transferred in pear shape bottle, in 0.8～1.0Mpa, 50～80 ℃ of situations, vacuumized 2h, obtain colourless or micro-yellow viscous fluid and be modified glutaraldehyde tanning agent.
Embodiment 3
(1) 170 parts of 150 parts of glutaraldehyde and ethylene glycol are added respectively in reactor, logical reflux condensation mode water, after stirring, adds 15 parts of thanomins to make its pH value between 7～9, is warming up to 80～90 ℃, insulation reaction 2～3h;
(2) in above-mentioned solution, add 180 parts, formaldehyde, and add 8 parts of thanomins to make its pH value between 8～10, be warming up to 90～100 ℃, insulation reaction 2～3h;
(3) be cooled to 70～80 ℃, add 15 parts of formic acid to make its pH value between 3～5, insulation reaction 2～3h;
(4) above-mentioned solution is transferred in pear shape bottle, in 0.8～1.0Mpa, 50～80 ℃ of situations, vacuumized 2h, obtain colourless or micro-yellow viscous fluid and be modified glutaraldehyde tanning agent.
Embodiment 4
(1) 160 parts of 145 parts of glutaraldehyde and ethylene glycol are added respectively in reactor, logical reflux condensation mode water, after stirring, adds 10 parts, sodium carbonate to make its pH value between 7～9, is warming up to 80～90 ℃, insulation reaction 2～3h;
(2) in above-mentioned solution, add 200 parts, formaldehyde, and add 7 parts, sodium carbonate to make its pH value between 8～10, be warming up to 90～100 ℃, insulation reaction 2～3h;
(3) be cooled to 70～80 ℃, add 8 parts of hydrochloric acid to make its pH value between 3～5, insulation reaction 2～3h;
(4) above-mentioned solution is transferred in pear shape bottle, in 0.8～1.0Mpa, 50～80 ℃ of situations, vacuumized 2h, obtain colourless or micro-yellow viscous fluid and be modified glutaraldehyde tanning agent.
Embodiment 5
(1) 165 parts of 125 parts of glutaraldehyde and ethylene glycol are added respectively in reactor, logical reflux condensation mode water, after stirring, adds 12 parts, salt of wormwood to make its pH value between 7～9, is warming up to 80～90 ℃, insulation reaction 2～3h;
(2) in above-mentioned solution, add 180 parts, formaldehyde, and add 7 parts, salt of wormwood to make its pH value between 8～10, be warming up to 90～100 ℃, insulation reaction 2～3h;
(3) be cooled to 70～80 ℃, add 6 parts of phosphoric acid to make its pH value between 3～5, insulation reaction 2～3h;
(4) above-mentioned solution is transferred in pear shape bottle, in 0.8～1.0Mpa, 50～80 ℃ of situations, vacuumized 2h, obtain colourless or micro-yellow viscous fluid and be modified glutaraldehyde tanning agent.
Embodiment 6
(1) 150 parts of 140 parts of glutaraldehyde and ethylene glycol are added respectively in reactor, logical reflux condensation mode water, after stirring, adds 10 parts of triethylamines to make its pH value between 7～9, is warming up to 80～90 ℃, insulation reaction 2～3h;
(2) in above-mentioned solution, add 175 parts, formaldehyde, and add 3 parts of triethylamines to make its pH value between 8～10, be warming up to 90～100 ℃, insulation reaction 2～3h;
(3) be cooled to 70～80 ℃, add 15 parts of oxoethanoic acids to make its pH value between 3～5, insulation reaction 2～3h;
(4) above-mentioned solution is transferred in pear shape bottle, in 0.8～1.0Mpa, 50～80 ℃ of situations, vacuumized 2h, obtain colourless or micro-yellow viscous fluid and be modified glutaraldehyde tanning agent.
Embodiment 7
(1) 180 parts of 120 parts of glutaraldehyde and ethylene glycol are added respectively in reactor, logical reflux condensation mode water, after stirring, adds 15 parts, salt of wormwood to make its pH value between 7～9, is warming up to 80～90 ℃, insulation reaction 2～3h;
(2) in above-mentioned solution, add 190 parts, formaldehyde, and add 9 parts, salt of wormwood to make its pH value between 8～10, be warming up to 90～100 ℃, insulation reaction 2～3h;
(3) be cooled to 70～80 ℃, add 20 parts, phenylformic acid to make its pH value between 3～5, insulation reaction 2～3h;
(4) above-mentioned solution is transferred in pear shape bottle, in 0.8～1.0Mpa, 50～80 ℃ of situations, vacuumized 2h, obtain colourless or micro-yellow viscous fluid and be modified glutaraldehyde tanning agent.
It should be noted that: the above-mentioned case study on implementation of the present invention is all that residual formaldehyde amount reaches seldom, shrinkage temperature is high and flexibility good in order to allow, and those skilled in the art can accomplish according to the method steps of case study on implementation.Reason is, the method of a lot of modified glutaraldehydes was all directly with formaldehyde, to carry out modification in the past, so be that formaldehyde residual in glutaraldehyde solution after modification or tanned finished product is all many, and after processing by method of modifying of the present invention, first spent glycol and glutaraldehyde are to react under alkaline condition in pH value, obtain protecting the glutaraldehyde after aldehyde radical, with formaldehyde, it is carried out to modification again, then in pH value, be to carry out deprotection under acidic conditions, finally vacuumize, just obtain novel modified glutaraldehyde, by the glutaraldehyde tanning agent after the method modification, shrinkage temperature raises and the good effect of flexibility, free formaldehyde is few, irritating smell is little, flexibility is good, can make finished leather pure white flexibly, plentiful, soft, high resilience, and water-fastness, sweat proof, physical strength strengthens, there is more excellent performance, this is also valuable point of the present invention.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a modified glutaraldehyde tanning agent, it is characterized in that, its raw material comprises: in parts by weight, 100-300 part glutaraldehyde, 50-200 part ethylene glycol, 100-300 part formaldehyde, 1-50 part are for regulating the alkaline matter, 1-50 part of pH value for regulating the acidic substance of pH value;
Described modified glutaraldehyde tanning agent is prepared by the following method:
Respectively glutaraldehyde and ethylene glycol are joined in reactor, be mixed to get the first mixture;
In described reactor, add for regulating the alkaline matter of pH value, regulating pH value is 7-9;
Described inside reactor is warming up to 80-90 ℃, and is incubated in the first setting-up time, obtain the first product;
In described the first product, add formaldehyde, and described for regulating the alkaline matter of pH value to adding in described reactor, and adjusting pH value is 8-10;
Described inside reactor is warming up to 90-100 ℃, and is incubated in the second setting-up time, obtain the second product;
Described inside reactor is cooled to 70-80 ℃, and adds for regulating the acidic substance of pH value in described reactor, regulate pH value to 3-5, and be incubated in the 3rd setting-up time, obtain third product;
Described third product is vacuumized and obtains modified glutaraldehyde tanning agent.
2. modified glutaraldehyde tanning agent according to claim 1, it is characterized in that, described raw material comprises: in parts by weight, described in the described glutaraldehyde of 110-150 part, the described ethylene glycol of 80-180 part, the described formaldehyde of 110-200 part, 5-20 part for regulating described in the alkaline matter, 5-20 part of pH value for regulating the acidic substance of pH value.
3. modified glutaraldehyde tanning agent according to claim 1 and 2, is characterized in that, described for regulate the alkaline matter of pH value comprise following one or more: sodium carbonate, salt of wormwood, sodium hydroxide, triethylamine, thanomin.
4. modified glutaraldehyde tanning agent according to claim 3, is characterized in that, when described, when regulating the alkaline matter of pH value to comprise sodium hydroxide, the mass percent concentration of described sodium hydroxide is 30%.
5. modified glutaraldehyde tanning agent according to claim 1 and 2, is characterized in that, described for regulate the acidic substance of pH value comprise following one or more: hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, phenylformic acid, oxoethanoic acid.
6. a preparation method for the modified glutaraldehyde tanning agent described in claim 1-5 any one, is characterized in that, comprising:
Respectively glutaraldehyde and ethylene glycol are joined in reactor, be mixed to get the first mixture;
In described reactor, add for regulating the alkaline matter of pH value, regulating pH value is 7-9;
Described inside reactor is warming up to 80-90 ℃, and is incubated in the first setting-up time, obtain the first product;
In described the first product, add formaldehyde, and described for regulating the alkaline matter of pH value to adding in described reactor, and adjusting pH value is 8-10;
Described inside reactor is warming up to 90-100 ℃, and is incubated in the second setting-up time, obtain the second product;
Described inside reactor is cooled to 70-80 ℃, and adds for regulating the acidic substance of pH value in described reactor, regulate pH value to 3-5, and be incubated in the 3rd setting-up time, obtain third product;
Described third product is vacuumized and obtains modified glutaraldehyde tanning agent.
7. preparation method according to claim 6, is characterized in that,
The described condition vacuumizing is 0.8-1.0Mpa, 50-80 ℃.
8. preparation method according to claim 6, is characterized in that,
Described described third product is vacuumized obtain modified glutaraldehyde tanning agent before, described preparation method also comprises: the gas backstreaming that the mode by condensing reflux produces while making to obtain described the first product and/or described the second product and/or described third product.
9. preparation method according to claim 6, is characterized in that,
Described the first setting-up time and/or described the second setting-up time and/or described the 3rd setting-up time are 2-3 hour.
10. the purposes of the modified glutaraldehyde tanning agent described in claim 1-5 any one, is characterized in that, for the pretan of white leather, main tanning and/or retanning, or the pretan of fur, main tanning and/or retanning.
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| CN107022655A (en) * | 2017-06-15 | 2017-08-08 | 泉州鑫彩贸易有限公司 | Tanning agent and its dogskin process for tanning for dogskin |
| CN107099625A (en) * | 2017-06-15 | 2017-08-29 | 泉州鑫彩贸易有限公司 | Tanning agent and its horse skin process for tanning for horse skin |
| CN107099624A (en) * | 2017-06-15 | 2017-08-29 | 泉州鑫彩贸易有限公司 | Tanning agent and its pigskin process for tanning for pigskin |
| CN107090527A (en) * | 2017-06-15 | 2017-08-25 | 泉州鑫彩贸易有限公司 | Tanning agent and its crocodile skin process for tanning for crocodile skin |
| CN106995861A (en) * | 2017-06-15 | 2017-08-01 | 泉州鑫彩贸易有限公司 | Tanning agent and its grey squirrel process for tanning for grey squirrel |
| CN107419039A (en) * | 2017-06-15 | 2017-12-01 | 泉州鑫彩贸易有限公司 | Tanning agent and its donkey hide process for tanning for donkey hide |
| CN107419040A (en) * | 2017-06-15 | 2017-12-01 | 泉州鑫彩贸易有限公司 | Tanning agent and its ox-hide process for tanning for ox-hide |
| CN107190108A (en) * | 2017-06-15 | 2017-09-22 | 泉州鑫彩贸易有限公司 | Tanning agent and its lynx process for tanning for lynx |
| CN107034324A (en) * | 2017-06-15 | 2017-08-11 | 泉州鑫彩贸易有限公司 | Tanning agent and its sheepskin process for tanning for sheepskin |
| CN107058648A (en) * | 2017-06-15 | 2017-08-18 | 泉州鑫彩贸易有限公司 | Tanning agent and its fox skin process for tanning for fox skin |
| CN108823339B (en) * | 2018-06-28 | 2021-01-29 | 武汉辅创科技有限公司 | Preparation method of environment-friendly modified aldehyde product |
| CN109207655B (en) * | 2018-08-22 | 2020-12-29 | 湖北微控生物科技有限公司 | Preparation method of environment-friendly modified glutaraldehyde leather tanning agent |
| CN109880940A (en) * | 2019-04-02 | 2019-06-14 | 四川达威科技股份有限公司 | Leather tanning agent, leather tanning method, leather and its dress ornament |
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