CN109535444A - The bleaching process of hydroxyethyl cellulose - Google Patents
The bleaching process of hydroxyethyl cellulose Download PDFInfo
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- CN109535444A CN109535444A CN201811454498.3A CN201811454498A CN109535444A CN 109535444 A CN109535444 A CN 109535444A CN 201811454498 A CN201811454498 A CN 201811454498A CN 109535444 A CN109535444 A CN 109535444A
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- hydroxyethyl cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
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Abstract
The present invention relates to the bleaching process of hydroxyethyl cellulose, belong to cellulose and chemical material technical field.Present invention solves the technical problem that be current hydroxyethyl cellulose bleaching effect it is bad, after bleaching viscosity reduce it is more.The invention discloses the bleaching process of hydroxyethyl cellulose, first piece alkali is dissolved in a solvent in the reaction vessel, open stirring, then stabilizer is added, hydroxyethyl cellulose is added after stabilizer dispersing and dissolving, after hydroxyethyl cellulose dispersion, hydrogen peroxide heating is added to be bleached, cool down after bleaching, being neutralized to PH with acid is 6.0~7.0, the product after discharging after washing, centrifugation, drying, crushing are bleached.The present invention develops a kind of novel bleaching process, has a significant effect to the bleaching of hydroxyethyl cellulose, while the viscosity reduction of hydroxyethyl cellulose is less, plays biggish facilitation for the quality-improving of daily use chemicals, coating products.
Description
Technical field
The invention belongs to cellulose and chemical material technical fields, and in particular to the bleaching process of hydroxyethyl cellulose.
Background technique
Hydroxyethyl cellulose (HEC) is by cotton fiber, through non-ionic fibre made of the processes such as alkalization, ethylene oxide etherification
The single ether of dimension element, since it has not, the non-ionic feature good with positive and negative ion effect, compatibility, HEC can be used as cladding
Agent, binder, cement and gypsum auxiliary agent, thickener, suspending agent, pharmaceutic adjuvant, antifoggant, fracturing fluid, gelling agent, waterproof
Agent etc. is widely used in the fields such as coating, petroleum, building, daily-use chemical industry, high molecular polymerization and textile industry.
Due to the fast development of coating, daily chemical products, market, which does not require nothing more than it, will excellent service performance, but also right
Its appearance has strict requirements, especially daily use chemicals and interior paint high-end product, and the whiteness of product is the weight for influencing appearance
Want factor, and hydroxyethyl ether cellulose (HEC) addition raw material important as its have the whiteness index of coating, daily chemical products
Have important influence, therefore, prepare whiteness meet client needs HEC it is most important.This hair is using hydrogen peroxide to life
More yellow product is bleached during producing, and can promote product quality, reduces the loss of waste material in production process.
The bleaching agent for being usually used in HEC bleaching has a sodium hypochlorite and hydrogen peroxide, when sodium hypochlorite bleaching HEC, bleaching effect compared with
Difference, and the ash content of product and gel particle increase after bleaching.When hydrogen peroxide bleaches HEC, due to hydrogen peroxide have compared with
Strong oxidation, the viscosity of product can reduce more when bleaching, and therefore, sodium hypochlorite and hydrogen peroxide bleaching effect are bad, i.e.,
For the bleaching of HEC product, there are no effective technologies at present.
Summary of the invention
Present invention solves the technical problem that being bad for the bleaching effect of hydroxyethyl cellulose at present, viscosity drop after bleaching
It is low more.
Technical proposal that the invention solves the above-mentioned problems is to provide the bleaching process of hydroxyethyl cellulose, including walks as follows
It is rapid:
First piece alkali is dissolved in a solvent in the reaction vessel, opens stirring, stabilizer is then added, stabilizer dispersion is molten
Hydroxyethyl cellulose is added after solution, after hydroxyethyl cellulose dispersion, hydrogen peroxide heating is added and is bleached, drops after bleaching
Temperature, being neutralized to PH with acid is 6.0~7.0, the product after discharging after washing, centrifugation, drying, crushing are bleached.
Wherein, piece alkali and solvent quality ratio are 0.1%~0.4%, and the mass ratio of piece alkali and hydroxyethyl cellulose is 0.5%
~2.5%, the mass ratio 2%~10% of hydrogen peroxide and hydroxyethyl cellulose.
Wherein, bleaching temperature is 45~75 DEG C, and bleaching time is 20~60 minutes.
Wherein, solvent is acetone.
Wherein, piece alkali is solid sodium hydroxide, mass percentage 98%.
Wherein, stabilizer is soluble magnesium salt, and the mass ratio with hydroxyethyl cellulose is 0.5%~2%.
Preferably, stabilizer is magnesium sulfate.
Beneficial effects of the present invention:
The present invention develops a kind of novel bleaching process, under the conditions of existing for highly basic, high temperature, the stabilizer, control one
Fixed technological parameter has a significant effect to the bleaching of hydroxyethyl cellulose, and the viscosity of hydroxyethyl cellulose reduces after bleaching
It is less.
Figure of description
Fig. 1 is hydroxyethyl cellulose bleaching front and back comparison diagram, and a is before bleaching, and b is after bleaching.
Specific embodiment
Hydrogen peroxide has stronger blanching effect for fiber, and the bleaching mechanism about hydrogen peroxide has following two saying:
1) saying is considered that decomposing hydrogen dioxide solution generates nascent oxygen (O) and has blanching effect: H to cellulose earlier2O2→
H2O+(O)；But present scientific research proves that nascent oxygen (O) energy oxycellulose especially under highly basic, high temperature causes its damage
Wound, but there are much effects to have no sufficient evidence bleaching.
2) what is widely quoted both at home and abroad at present is the argument of German Bi Tenai (Peter Nay): decomposing hydrogen dioxide solution thinks to lead
Causing fiber bleached substance is hydrogen peroxide ions HOO-, and the main substance of cellulose oxidation is caused to be hydrogen peroxide freedom
Base HOO, therefore to inhibit in bleaching process the generation of HOO, and make HOO-It stably generates, prevents from cellulose in this way
Oxidation, to obtain good bleaching effect.In aqueous solution, dioxygen hydrolytic dissociation generates HOO?, i.e. H2O2→H++HOO?.In water
Dissociation constant K20=1.78 × 10- 12, HOO as can be seen from the above equation?Amount with solution ph increase and increase, and bleach be
It is carried out under alkaline condition.But as alkali concentration increases, hydrogen peroxide, which can decompose, generates excessive HOO and HO free radical,
Since free radical has great activity, although having bleaching effect to cellulose, free radical excessively easily makes cellulose
Damage.Therefore, effective stabilizer must be added in bleaching liquid, to inhibit to generate excessive free radical due to catalytic decomposition,
Increase HOO simultaneously?Content, to prevent HEC product oxidative degradation, and then play preferable blanching effect.HOO?With fiber
Oxidation reaction occurs for pigment, has bleaching, colour killing, impurity elimination effect.Reaction equation is as follows:
Based on above-mentioned analysis, the present invention provides the bleaching process of hydroxyethyl cellulose, specifically comprises the following steps:
First piece alkali is dissolved in a solvent in the reaction vessel, opens stirring, stabilizer A, stabilizer A dispersion is then added
Hydroxyethyl cellulose is added after dissolution, after hydroxyethyl cellulose dispersion, is eventually adding hydrogen peroxide and is warming up to certain temperature progress
Bleaching, insulated and stirred certain time are cooled to 30 DEG C, and being neutralized to PH with acid is 6.0~7.0, through washing, centrifugation, baking after discharging
It does, crush the product after being bleached.
Wherein, piece alkali and solvent quality ratio are 0.1%~0.4%, and the mass ratio of piece alkali and hydroxyethyl cellulose is 0.5%
~2.5%, the mass ratio 2%~10% of hydrogen peroxide and hydroxyethyl cellulose.
Wherein, 45~75 DEG C of bleaching temperature, soaking time 20~60 minutes.
Wherein, solvent is preferably acetone.
Wherein, piece alkali is preferably solid sodium hydroxide, mass percentage 98%.
Wherein, stabilizer is soluble magnesium salt, and the mass ratio with hydroxyethyl cellulose is 0.5%~2%.
Preferably, stabilizer is magnesium sulfate.
It is can also be applied to the bleaching of other cellulose derivatives.
The present invention will be further explained by the following examples and explanation.
The color for the hydroxyethyl cellulose product selected in embodiment is more yellow, whiteness 54, viscosity be 493mpa.s (2%,
25 DEG C, LVT), hydrogen peroxide concentration is 27.5% (m/m), and stabilizer used is magnesium sulfate.
Embodiment 1
560g solvent, 0.56g piece alkali are weighed, uses solvent solution tablet alkali in the reaction vessel, opens stirring, it is steady that 0.5g is added
Determine agent, 100g hydroxyethyl cellulose is added after stabilizer dispersing and dissolving and is eventually adding 2g dioxygen after hydroxyethyl cellulose dispersion
Water is warming up to 45 DEG C, insulated and stirred 30min.30 DEG C are cooled to, being neutralized to PH with acid is 6.0~7.0.It is carried out after centrifugation with solvent
Washing, the product PHEC-1 after centrifugation, drying, crushing are bleached, the performance data of products obtained therefrom are shown in Table 1.It is obtained by example 1
Out, product whiteness is increased to 64 by 54, improves 18.5% before relatively bleaching.
Table 1
| Lot number | Whiteness | Viscosity (2%, 25 DEG C, LVT) mpa.s |
| HEC (before bleaching) | 54 | 493 |
| PHEC-1 | 64 | 489 |
Embodiment 2
560g solvent, 1.12g piece alkali are weighed, uses solvent solution tablet alkali in the reaction vessel, opens stirring, 1g is added and stablizes
Agent adds 100g hydroxyethyl cellulose after stabilizer dispersing and dissolving and is eventually adding 6g hydrogen peroxide after hydroxyethyl cellulose dispersion
60 DEG C are warming up to, insulated and stirred 30min.30 DEG C are cooled to, being neutralized to PH with acid is 6.0~7.0.It is washed after centrifugation with solvent
It washs, the product PHEC-2 after centrifugation, drying, crushing are bleached.The performance data of products obtained therefrom is shown in Table 2, and bleaching front and back is right
It is more as shown in Figure 1 than scheming.It can show that product whiteness is increased to 78 by 54, and product whiteness improves 44.4% by 2 data of example.
Table 2
Embodiment 3
560g solvent, 2.24g piece alkali are weighed, uses solvent solution tablet alkali in the reaction vessel, opens stirring, 2g is added and stablizes
Agent adds 100g hydroxyethyl cellulose after stabilizer dispersing and dissolving and is eventually adding 8g hydrogen peroxide after hydroxyethyl cellulose dispersion
60 DEG C are warming up to, insulated and stirred 30min.30 DEG C are cooled to, being neutralized to PH with acid is 6.0~7.0.It is washed after centrifugation with solvent
It washs, the product PHEC-3 after centrifugation, drying, crushing are bleached, the performance data of products obtained therefrom is shown in Table 3.By 3 data of example
It can obtain, product whiteness is increased to 77 by 54, and product whiteness improves 42.6%.
Table 3
| Lot number | Whiteness | Viscosity (2%, 25 DEG C, LVT) mpa.s |
| HEC (before bleaching) | 54 | 493 |
| PHEC-3 | 77 | 386 |
Embodiment 4
Weigh 560g solvent, 2.24g piece alkali, in the reaction vessel use solvent solution tablet alkali, open stirring, be added 100g compared with
Yellow hydroxyethyl cellulose is eventually adding 6g hydrogen peroxide and is warming up to 60 DEG C after hydroxyethyl cellulose dispersion, insulated and stirred 30min.
30 DEG C are cooled to, being neutralized to PH with acid is 6.0-7.0.It is washed after centrifugation with solvent, is floated through centrifugation, drying, crushing
Product PHEC-4 after white.Example 4 and the difference of example 3 are that example 4 is not added with stabilizer.The performance data of products obtained therefrom is shown in Table
4, it is obtained by example 4, product whiteness improves 7%, and product is still more yellow, and the viscosity reduction of product is more.
Table 4
| Lot number | Whiteness | Viscosity (2%, 25 DEG C, LVT) mpa.s |
| HEC (before bleaching) | 54 | 493 |
| PHEC-4 | 58 | 36 |
Claims (6)
1. the bleaching process of hydroxyethyl cellulose, it is characterised in that include the following steps: in the reaction vessel first by piece alkali molten
It is dissolved in agent, opens stirring, stabilizer is then added, hydroxyethyl cellulose is added after stabilizer dispersing and dissolving, ethoxy is fine
After dimension element dispersion, hydrogen peroxide heating is added and is bleached, cools down after bleaching, being neutralized to PH with acid is 6.0~7.0, discharging
Product after being bleached by washing, centrifugation, drying, crushing.
2. the bleaching process of hydroxyethyl cellulose according to claim 1, it is characterised in that: described alkali and solvent quality
Than being 0.1%~0.4%, the mass ratio of piece alkali and hydroxyethyl cellulose is 0.5%~2.5%, hydrogen peroxide and hydroxy ethyl fiber
The mass ratio of element is 2%~10%.
3. the bleaching process of hydroxyethyl cellulose according to claim 1 or 2, it is characterised in that: the bleaching temperature is
45~75 DEG C, bleaching time is 20~60 minutes.
4. the bleaching process of described in any item hydroxyethyl celluloses according to claim 1~3, it is characterised in that: described alkali
For solid sodium hydroxide, mass percentage 98%.
5. the bleaching process of hydroxyethyl cellulose according to any one of claims 1 to 4, it is characterised in that: the stabilization
Agent is soluble magnesium salt, and the mass ratio with hydroxyethyl cellulose is 0.5%~2%.
6. the bleaching process of described in any item hydroxyethyl celluloses according to claim 1~5, it is characterised in that: the stabilization
Agent is magnesium sulfate.
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| CN201811454498.3A CN109535444B (en) | 2018-11-30 | 2018-11-30 | Bleaching process of hydroxyethyl cellulose |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115746151A (en) * | 2022-11-21 | 2023-03-07 | 泸州北方纤维素有限公司 | Bleaching process of ethyl cellulose |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115746151A (en) * | 2022-11-21 | 2023-03-07 | 泸州北方纤维素有限公司 | Bleaching process of ethyl cellulose |
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