CN106367943A - Preparation method of low-temperature hydrogen peroxide activating agent - Google Patents
Preparation method of low-temperature hydrogen peroxide activating agent Download PDFInfo
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- CN106367943A CN106367943A CN201610825229.8A CN201610825229A CN106367943A CN 106367943 A CN106367943 A CN 106367943A CN 201610825229 A CN201610825229 A CN 201610825229A CN 106367943 A CN106367943 A CN 106367943A
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- China
- Prior art keywords
- hydrogen peroxide
- epoxychloropropane
- carbamide
- tin tetrafluoride
- activating agent
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Abstract
The invention provides a preparation method of a low-temperature hydrogen peroxide activating agent. The preparation method is characterized by comprising the following steps that 1, urea and ethyl alcohol are added to a three-mouth flask, tin tetrafluoride is added at a time after the urea is dissolved, even stirring is performed, then epoxy chloropropane is dropwise added to the three-mouth flask, the mole ratio of the epoxy chloropropane to the urea to the tin tetrafluoride is 5-10 to 2-12 to 1, reaction is performed at the temperature of 60-85 DEG C for 5-7 hours after adding is dropwise completed, and the adding weight of the ethyl alcohol is not smaller than the total adding weight of the epoxy chloropropane, the urea and the tin tetrafluoride; 2, reduced pressure distillation is performed under the conditions of 55 DEG C and -0.1 MPa to remove ethyl alcohol, unreacted epoxy chloropropane and other by-products, then the residual product in the reaction container is dissolved by using methyl alcohol, a filter membrane of 100 microns is used for filtering out insoluble impurities, filtrate is distilled under the conditions of 30 DEG C and -0.1 MPa to remove methyl alcohol, and drying is performed at the temperature of 50 DEG C to obtain the low-temperature hydrogen peroxide activating agent white crystal. By the adoption of the activating agent, the fiber damage is decreased, and the production efficiency is improved on the basis that the yarn whiteness and the capillary effect are kept equivalent to conventional scouring and bleaching.
Description
Technical field
The present invention relates to dyeing cotton fiber pre-treatment field is and in particular to a kind of preparation of low temperature Activation of Hydrogen Peroxide Solution agent
Method.
Background technology
Natural cotton fiber is internal often to contain natural pigment, pectin, ash grade impurity, the capillary effect of impact fiber and whiteness, enter
And easily cause dyestuff and fabric finishing agent skewness.Textile printing and dyeing factory is usually used bleach and removes yarn interior impurity.
Hydrogen peroxide is a kind of bleaching agent for unchlorine commonly using in textile industry, can be used for cellulose fibre, protein fibre and its with
The bleaching of chemical fibre blend fabric.But, traditional hydrogen peroxide bleaching process needs in high temperature, highly basic, long time treatment bar
Optimal bleaching effect could be obtained under part.And the degraded of this condition meeting accelerating fibers, cause the damage of fiber, cause strength
Reduce.And higher treatment temperature increased energy resource consumption, do not meet the trend of energy-conserving and environment-protective.
Content of the invention
The present invention is directed to the high energy consumption that current pre-treating technology exists, time-consuming problem, provides a kind of low temperature hydrogen peroxide to live
The preparation method of agent.Its technical scheme is:
A kind of preparation method of low temperature Activation of Hydrogen Peroxide Solution agent is it is characterised in that adopt following steps:
1) add carbamide and ethanol in equipped with constant pressure funnel, thermometer, the there-necked flask of agitating device, treat that carbamide dissolves
Disposably add tin tetrafluoride afterwards, stir, then use constant pressure funnel Deca epoxychloropropane in there-necked flask, epoxy chlorine
The mol ratio of propane, carbamide and tin tetrafluoride is 5～10:2～12:1, and the time for adding of wherein epoxychloropropane controls in 1-
2h, after being added dropwise to complete, 60-85 DEG C of reaction 5-7h, the addition weight of ethanol is not less than epoxychloropropane, carbamide and tin tetrafluoride
Total addition weight；
2) after reaction terminates, in 55 DEG C, -0.1mpa vacuum distillation removing ethanol, unreacted epoxychloropropane and other
By-product, then with resultant product in methanol dissolving reaction vessel, filters off insoluble impurity with 100 μm of filter membranes, filtrate 30 DEG C ,-
After 0.1mpa distillation for removing methanol, dry to obtain low temperature Activation of Hydrogen Peroxide Solution agent white crystal for 50 DEG C.
Object of the present invention be used for process at low temperature in refining, concise with the routine of existing like product compared with, have following excellent
Point:
1) reducing energy consumption.Concise for traditional cheese temperature is down to 70 DEG C by 105 DEG C, with routine concise compared with, energy consumption drop
Low by nearly 40%, energy-conserving action is notable.
2) time-consuming.After temperature reduces, rise gentle temperature fall time and reduce (about reducing total duration 25%), efficiency is carried
High.
3) after reducing concise temperature, cellulose damage degree substantially reduces, and decreases the generation of cellulose sodium salt, mitigates sewage
Processing load.
4) the Activation of Hydrogen Peroxide Solution agent that the method is obtained, can be reacted with hydrogen peroxide under cryogenic, and generation has higher
The high activity imines peroxide acid anion of reduction potential, can aoxidize the purpose that the impurity such as pigment reach colour killing under cryogenic,
Solve the deficiencies in the prior art.
Specific embodiment
Below by way of specific embodiment, the invention will be further described.
Embodiment one concretely comprises the following steps:
1) add 6g carbamide and 25g ethanol in equipped with constant pressure funnel, thermometer, the there-necked flask of agitating device, wait to urinate
Disposably add 3g tin tetrafluoride after element dissolving and stir, then uniformly dripped in there-necked flask in 1h with constant pressure funnel
Plus 15g epoxychloropropane, it is added dropwise to complete rear system and heat up and control temperature 60 C, response time 5h.
2) after reaction terminates, in 55 DEG C, -0.1mpa vacuum distillation removing ethanol, unreacted epoxychloropropane and other
By-product, then uses resultant product in 300ml methanol dissolving reaction vessel, and 100 μm of filter membranes filter off insoluble impurity, and filtrate is 30
DEG C, after -0.1mpa distillation for removing methanol, dry to obtain No. 1 low temperature Activation of Hydrogen Peroxide Solution agent whiteness crystal for 50 DEG C.
Embodiment two concretely comprises the following steps:
1) add 36g carbamide and 70g ethanol in equipped with constant pressure funnel, thermometer, the there-necked flask of agitating device, wait to urinate
Disposably add 3g tin tetrafluoride after plain dissolving and stir, then use constant pressure funnel uniform in there-necked flask in 1.5h
Deca 30g epoxychloropropane, is added dropwise to complete rear system and heats up and control temperature 70 C, response time 6h.
2) after reaction terminates, in 55 DEG C, -0.1mpa vacuum distillation removing ethanol, unreacted epoxychloropropane and other
By-product, then uses resultant product in 1.5l methanol dissolving reaction vessel, and 100 μm of filter membranes filter off insoluble impurity, and filtrate is 30
DEG C, after -0.1mpa distillation for removing methanol, dry to obtain No. 2 low temperature Activation of Hydrogen Peroxide Solution agent whiteness crystal for 50 DEG C.
Embodiment three concretely comprises the following steps:
1) add 20g carbamide and 50g ethanol in equipped with constant pressure funnel, thermometer, the there-necked flask of agitating device, wait to urinate
Disposably add 3g tin tetrafluoride after plain dissolving and stir, then use constant pressure funnel uniform in there-necked flask in 1.5h
Deca 25g epoxychloropropane, is added dropwise to complete rear system and heats up and control temperature 70 C, response time 6h.
2) after reaction terminates, in 55 DEG C, -0.1mpa vacuum distillation removing ethanol, unreacted epoxychloropropane and other
By-product, then uses resultant product in 1l methanol dissolving reaction vessel, and 100 μm of filter membranes filter off insoluble impurity, filtrate 30 DEG C ,-
After 0.1mpa distillation for removing methanol, dry to obtain No. 3 low temperature Activation of Hydrogen Peroxide Solution agent whiteness crystal for 50 DEG C.
Example IV concretely comprises the following steps:
1) add 10g carbamide and 40g ethanol in equipped with constant pressure funnel, thermometer, the there-necked flask of agitating device, wait to urinate
Disposably add 3g tin tetrafluoride after plain dissolving and stir, then use constant pressure funnel uniform in there-necked flask in 1.5h
Deca 20g epoxychloropropane, is added dropwise to complete rear system and heats up and control 80 DEG C of temperature, response time 7h.
2) after reaction terminates, in 55 DEG C, -0.1mpa vacuum distillation removing ethanol, unreacted epoxychloropropane and other
By-product, then uses resultant product in 500ml methanol dissolving reaction vessel, and 100 μm of filter membranes filter off insoluble impurity, and filtrate is 30
DEG C, after -0.1mpa distillation for removing methanol, dry to obtain No. 4 low temperature Activation of Hydrogen Peroxide Solution agent whiteness crystal for 50 DEG C.
Using above-mentioned four kinds of low temperature Activation of Hydrogen Peroxide Solution agent, process Quality Pure Cotton Yarn Production with refining agent, sodium hydroxide, hydrogen peroxide one bath
Line, and contrasted with conventional refining process, Ju Ti Pei Fang is shown in Table 1.
Table 1:
| Formula using Activation of Hydrogen Peroxide Solution agent of the present invention | Consumption | Using conventional concise formula | Consumption |
| Scouring agent | 2.0g/l | Scouring agent | 2.0g/l |
| Caustic soda (48 ° of b é) | 3.0g/l | Caustic soda (48 ° of b é) | 3.0g/l |
| h2o2(27.5%) | 10g/l | h2o2(27.5%) | 10g/l |
| Activation of Hydrogen Peroxide Solution agent | 1g/l | Activation of Hydrogen Peroxide Solution agent | 1g/l |
Compliance test result process is as follows: 10g yarn is immersed in the body lotion that the above-mentioned formula of 100g is prepared, then will contain yarn
The body lotion of line is to slowly warm up to 70 DEG C (common process is for 105 DEG C) with the speed of 2.5 DEG C/min, is processed with infrared dyeing machine
40min；After process, 70 DEG C of 500ml clear water of yarn washs 10min, then washs 5min, Ran Houyong with 50 DEG C of 500ml clear water
After 500ml clear water washing 5min under room temperature, dry 4 minutes in 105 DEG C in baking oven.The whiteness of yarn after test processes, strongly
And capillary effect.The performance comparison of embodiment 1-4 gained activator refining process is shown in Table 2.
Table 2:
The present invention uses low temperature Activation of Hydrogen Peroxide Solution agent, builds hydrogen peroxide, the concise system of activator, using water bath processing side
Method, reaches the good bleaching effect to yarn, keeps the basis maintaining an equal level with conventional refining and bleaching in the whiteness making yarn and capillary effect
On, decrease the damage to fiber, reduce energy consumption, improve production efficiency, the ecological, environmental protective for dyeing and energy-saving
Significant.
Claims (1)
1. a kind of preparation method of low temperature Activation of Hydrogen Peroxide Solution agent is it is characterised in that adopt following steps:
1) carbamide and ethanol are added in equipped with constant pressure funnel, thermometer, the there-necked flask of agitating device, one after carbamide dissolving
Secondary property adds tin tetrafluoride, stirs, and then uses constant pressure funnel Deca epoxychloropropane, epoxy chloropropionate in there-necked flask
The mol ratio of alkane, carbamide and tin tetrafluoride is 5～10:2～12:1, and the time for adding of wherein epoxychloropropane controls in 1-2h,
After being added dropwise to complete, 60-85 DEG C of reaction 5-7h, the addition weight of ethanol is not less than the total of epoxychloropropane, carbamide and tin tetrafluoride
Add weight；
2) after reaction terminates, in 55 DEG C, -0.1mpa vacuum distillation removing ethanol, unreacted epoxychloropropane and other by-product
Thing, then with resultant product in methanol dissolving reaction vessel, filters off insoluble impurity with 100 μm of filter membranes, filtrate 30 DEG C ,-
After 0.1mpa distillation for removing methanol, dry to obtain low temperature Activation of Hydrogen Peroxide Solution agent white crystal for 50 DEG C.
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| CN201610825229.8A CN106367943B (en) | 2016-09-16 | 2016-09-16 | The preparation method of low temperature Activation of Hydrogen Peroxide Solution agent |
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| CN201610825229.8A CN106367943B (en) | 2016-09-16 | 2016-09-16 | The preparation method of low temperature Activation of Hydrogen Peroxide Solution agent |
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| CN106367943A true CN106367943A (en) | 2017-02-01 |
| CN106367943B CN106367943B (en) | 2018-03-27 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845744A (en) * | 2010-05-18 | 2010-09-29 | 广东德美精细化工股份有限公司 | Low-temperature scouring and bleaching assistant and preparation method and application thereof |
| CN103304481A (en) * | 2012-03-15 | 2013-09-18 | 广东德美精细化工股份有限公司 | Preparation method of low-temperature oxygen bleaching activator as well as scouring and bleaching formula and method thereof |
| CN103306129A (en) * | 2012-03-15 | 2013-09-18 | 广东德美精细化工股份有限公司 | Processing liquid and processing process for ultralow-temperature scouring and bleaching of cotton knitted fabric |
| CN103924437A (en) * | 2014-04-03 | 2014-07-16 | 东华大学 | Low-temperature activating bleaching agent for textile products, as well as preparation method and application of bleaching agent |
-
2016
- 2016-09-16 CN CN201610825229.8A patent/CN106367943B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845744A (en) * | 2010-05-18 | 2010-09-29 | 广东德美精细化工股份有限公司 | Low-temperature scouring and bleaching assistant and preparation method and application thereof |
| CN103304481A (en) * | 2012-03-15 | 2013-09-18 | 广东德美精细化工股份有限公司 | Preparation method of low-temperature oxygen bleaching activator as well as scouring and bleaching formula and method thereof |
| CN103306129A (en) * | 2012-03-15 | 2013-09-18 | 广东德美精细化工股份有限公司 | Processing liquid and processing process for ultralow-temperature scouring and bleaching of cotton knitted fabric |
| CN103924437A (en) * | 2014-04-03 | 2014-07-16 | 东华大学 | Low-temperature activating bleaching agent for textile products, as well as preparation method and application of bleaching agent |
Non-Patent Citations (2)
| Title |
|---|
| 杨栋樑等: "活化双氧水漂白体系新技术的近况(一)", 《印染》 * |
| 赵燕等: "3-氯-2-羟丙基脲的合成", 《精细化工》 * |
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