CN111892827A - Preparation method of reduced liquid indigo - Google Patents
Preparation method of reduced liquid indigo Download PDFInfo
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- CN111892827A CN111892827A CN202010785779.8A CN202010785779A CN111892827A CN 111892827 A CN111892827 A CN 111892827A CN 202010785779 A CN202010785779 A CN 202010785779A CN 111892827 A CN111892827 A CN 111892827A
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- reaction kettle
- indigo
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- reduced liquid
- reaction
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B7/00—Indigoid dyes
- C09B7/02—Bis-indole indigos
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0077—Preparations with possibly reduced vat, sulfur or indigo dyes
- C09B67/0078—Preparations of vat, sulfur or indigo dyes in liquid form
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- Organic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of reduced liquid indigo, which relates to the technical field of printing and dyeing and comprises the following steps: adding 650 parts of water into the reaction kettle, and starting stirring; controlling the stirring speed of the reaction kettle at 1000 revolutions per minute, and adding 5.0 parts of bleached BC powder, 70 parts of reducing agent, 80 parts of granular alkali and 195 parts of indigo into the reaction kettle within 30 minutes; controlling the stirring speed of the reaction kettle at 800 revolutions per minute, and sealing the reaction kettle for reaction for 20-30 minutes; sampling and detecting whether the reaction is sufficient or not, stopping stirring after the reaction is sufficient, and reducing the temperature of the obtained reduction liquid indigo to be below 30 ℃; and discharging the reducing liquid indigo from the reaction kettle, subpackaging the discharged reducing liquid indigo into a packaging container, and introducing nitrogen into the packaging container to perform isolation protection on the reducing liquid indigo. The invention has no potential safety hazard; the reaction period is short, and the productivity is high; no three wastes are discharged; according to the requirements of customers on color light, two dyes can be reduced simultaneously; the material performance is stable, and the dyed object has bright color.
Description
Technical Field
The invention relates to the technical field of printing and dyeing, in particular to a preparation method of reduced liquid indigo.
Background
Indigo is one of the oldest pigments known to man and is widely used in the food, pharmaceutical and printing industries, it is slightly soluble in water, ethanol, glycerol and propylene glycol and insoluble in fats and oils. The 0.05% aqueous solution is dark blue, 1g is soluble in about 100ml of water at 25 deg.C, and has lower solubility to water than other edible synthetic pigments, and the 0.05% aqueous solution is blue.
The traditional technology adopts hydrogenation reduction technology to produce reduced liquid indigo, which has the following defects:
1) hydrogen is used as a reducing agent, so that the hydrogen is easy to combust and explode, the destructive power is large, the potential safety hazard is high, the precision requirement of equipment is particularly high, and the safety measure investment is large;
2) expensive catalyst must be adopted, and the catalyst needs to be replaced and regenerated periodically, so that the loss of noble metal in the regeneration process and the catalytic reaction is large;
3) it is difficult to completely reduce both dyes under the same conditions;
4) when the generated pre-reduced indigo is used for dyeing, the color light of the dyed object is slightly grey and dark;
5) there is a discharge of three wastes.
Disclosure of Invention
The present invention aims to provide a process for the preparation of reduced liquid indigo, which alleviates the above problems.
In order to alleviate the above problems, the technical scheme adopted by the invention is as follows:
a preparation method of reduced liquid indigo comprises the following raw materials in parts by weight:
indigo blue: 195 parts of a binder;
bleaching blue BC powder: 5 parts of a mixture;
reducing agent: 70 parts of (B);
granular alkali: 80 parts of a mixture;
water: 650 parts of (B);
the preparation method comprises the following steps:
s1, adding 650 parts of water into the reaction kettle, and starting stirring;
s2, controlling the stirring speed of the reaction kettle at 1000 rpm, and adding 5.0 parts of bleached BC powder, 70 parts of reducing agent, 80 parts of granular alkali and 195 parts of indigo into the reaction kettle within 30 minutes;
s3, controlling the stirring speed of the reaction kettle at 800 revolutions per minute, and sealing the reaction kettle for reaction for 20-30 minutes;
s4, sampling from the reaction kettle, detecting, confirming whether the materials are fully reacted, if the reaction is not complete, executing a step S5, and if the reaction is complete, executing a step S6;
s5, after the materials in the reaction kettle react for 5 minutes, jumping to the step S4;
s6, cooling the reaction kettle to reduce the temperature of the reduced liquid indigo blue obtained in the reaction kettle to below 30 ℃;
and S7, discharging the reduced liquid indigo from the reaction kettle, subpackaging the discharged reduced liquid indigo into a packaging container, introducing nitrogen into the packaging container to perform isolation protection on the reduced liquid indigo, wherein the air pressure in the packaging container is greater than the external atmospheric pressure.
Further, the indigo in the raw material is powdery or granular.
Further, the content of sodium hydroxide in the granular alkali is more than or equal to 98.5 percent.
Furthermore, the content of effective components in the reducing agent is more than or equal to 99.0 percent, and the heat-resistant stability is more than 50 minutes under the condition of 95 +/-0.5.
Further, reation kettle is stainless steel double-layered cover reation kettle of volume 5m thin blooms, and its built-in dispersion impeller adjustable frequency, and its motor wiring mode is three-phase five-wire system, and operating voltage is 380V.
Furthermore, the reaction kettle is provided with a cold water cooling unit for cooling the internal materials, the cold water cooling unit can cool the materials in the reaction kettle to 4 ℃ at the lowest, and the cold water conveying amount of the cold water cooling unit is 200 Kg/h.
Further, in step S7, compressed air is prepared by using an air compression system with a compressed air amount of 210 cubic/hour, and the nitrogen gas is prepared by using a nitrogen production system.
Furthermore, the nitrogen production speed of the nitrogen production system is 10 cubic meters per hour, and the purity of the produced nitrogen is more than or equal to 99.0 percent.
Further, in step S7, the packaging container for separately storing the reduced liquid indigo is a tank or a ton drum.
Compared with the prior art, the invention has the beneficial effects that:
1) the reaction is carried out at normal temperature and normal pressure, flammable, explosive and dangerous chemicals are not used during production, flammable, explosive and toxic substances are not generated during production, and potential safety hazards do not exist;
2) the reaction period is short, and the productivity is high;
3) no three wastes are discharged;
4) according to the requirements of customers on color light, two dyes can be reduced simultaneously;
5) the material performance is stable, and the dyed object has bright color.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow chart of a method of preparing reduced liquid indigo according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, an embodiment of the present invention provides a method for preparing reduced liquid indigo, which finally completes production of 1.0 ton of reduced liquid indigo product, specifically as follows:
preparing materials:
indigo blue: 195 kg;
bleaching blue BC powder: 5.0 kg;
reducing agent: 70 kg;
granular alkali: 80 kg;
water: 650 kg.
Wherein, the indigo is powdery or granular; in the granular alkali, the content of sodium hydroxide is more than or equal to 98.5 percent; the content of active ingredients in the reducing agent is more than or equal to 99.0 percent, and the heat-resistant stability is more than 50 minutes under 95 +/-0.5; the strength of the blanched BC powder is more than or equal to 100 percent (compared with a standard product); the water needs to reach the standard of drinking water.
The equipment requirements used in the preparation process are as follows:
1. 5 cubic stainless steel jacket reation kettle
Built-in dispersion disc frequency modulation
Good grounding of the device
The motor wiring mode must be three-phase five-wire system, and the working voltage is 380V
2. Cold water cooling unit
The lowest temperature reduction is 4 DEG C
The amount of cold water transferred is 200Kg/h
3. Air compression system
Compressed air production amount 210 cubic/hour
4. Nitrogen making system
The purity of the produced nitrogen is more than or equal to 99 percent, and the produced nitrogen accounts for 10 cubic meters per hour;
the process for preparing reduced liquid indigo is as follows:
adding 650kg of water into the reaction kettle, and starting stirring;
controlling the stirring speed of the reaction kettle at 1000 revolutions per minute, and adding 5.0kg of bleached BC powder, 70kg of reducing agent, 80kg of granular alkali and 195kg of indigo into the reaction kettle within 30 minutes;
controlling the stirring speed of the reaction kettle at 800 revolutions per minute, sealing the reaction kettle for reaction for 20-30 minutes, and raising the temperature of materials in the kettle to 70-80 ℃ due to the reaction;
taking a sample from the reaction kettle, detecting, confirming whether the materials are fully reacted, if the reaction is not complete, continuing to stir for reaction, and if the reaction is complete, cooling the reaction kettle to reduce the temperature of the reduced liquid indigo obtained in the reaction kettle to below 30 ℃, and then obtaining 1.0 ton of reduced liquid indigo product;
discharging the reducing liquid indigo from the reaction kettle, subpackaging the discharged reducing liquid indigo into a packaging container, introducing nitrogen into the packaging container to carry out isolation protection on the reducing liquid indigo, wherein the internal air pressure of the packaging container is higher than the external atmospheric pressure and is micro-positive pressure.
In this embodiment, the packaging container is a tank or a ton drum.
In this embodiment, the sample obtained during sampling should satisfy the following conditions:
1. good appearance fluidity and no sediment;
2. the content of indigo in the product is more than or equal to 18.0 percent;
3. the dye-accelerating component is more than or equal to 5.0 percent.
The preparation process of the reduced liquid indigo is developed through multiple experiments and repeated demonstration including destructive experiments, and is already used for large-scale production. The obtained reduced liquid indigo product has good performance, the quality and the dosage of each raw material meet the following requirements, qualified products can be produced, and the use requirements of customers can be met. Compared with the prior art, the method has the following advantages:
1. the potential safety hazard problem is solved:
the production of the pre-reduced indigo blue by adopting the technology can be finished at normal temperature and normal pressure, flammable and explosive materials are not used during production, and toxic, harmful and flammable gases are not generated in the production process.
2. Solves the problem of three-waste discharge:
the pre-reduced indigo produced by adopting the technology does not produce waste water, waste gas and waste residue, fully embodies the advancement of the technology, and accords with the national green development concept.
3. The requirements of customers on the color of the dyed materials are met:
one or two dyes can be reduced under the same condition, which is beneficial to meeting different requirements of customers on color light and avoids the problems of grey and dark color of the dyed object.
4. The problem of partial precipitation of the indigo reducing solution is solved:
on one hand, the process has thorough reaction, and on the other hand, no matter in the product production or product packaging and transporting process, nitrogen is adopted for protection, and the product is not oxidized by air, so that the product has good fluidity and no sediment, and is smooth to use by users.
5. The method conforms to the national industrial adjustment policy of energy conservation, consumption reduction and high productivity:
the production of the pre-reduced indigo by the technical scheme can be finished by utilizing the self heat release of the reaction without supplementing energy, and the productivity can be adjusted at any time according to the capacity of the market and the requirements of customers.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of reduced liquid indigo is characterized in that the adopted raw materials comprise the following components in parts by weight:
indigo blue: 195 parts of a binder;
bleaching blue BC powder: 5 parts of a mixture;
reducing agent: 70 parts of (B);
granular alkali: 80 parts of a mixture;
water: 650 parts of (B);
the preparation method comprises the following steps:
s1, adding 650 parts of water into the reaction kettle, and starting stirring;
s2, controlling the stirring speed of the reaction kettle at 1000 rpm, and adding 5.0 parts of bleached BC powder, 70 parts of reducing agent, 80 parts of granular alkali and 195 parts of indigo into the reaction kettle within 30 minutes;
s3, controlling the stirring speed of the reaction kettle at 800 revolutions per minute, and sealing the reaction kettle for reaction for 20-30 minutes;
s4, sampling from the reaction kettle, detecting, confirming whether the materials are fully reacted, if the reaction is not complete, executing a step S5, and if the reaction is complete, executing a step S6;
s5, after the materials in the reaction kettle react for 5 minutes, jumping to the step S4;
s6, cooling the reaction kettle to reduce the temperature of the reduced liquid indigo blue obtained in the reaction kettle to below 30 ℃;
and S7, discharging the reduced liquid indigo from the reaction kettle, subpackaging the discharged reduced liquid indigo into a packaging container, introducing nitrogen into the packaging container to perform isolation protection on the reduced liquid indigo, wherein the air pressure in the packaging container is greater than the external atmospheric pressure.
2. The method for preparing reduced liquid indigo according to claim 1, wherein the indigo in the raw material is powdery or granular.
3. The process according to claim 1, wherein the content of sodium hydroxide in the granular alkali is not less than 98.5%.
4. The method for preparing reduced liquid indigo according to claim 1, wherein the content of the effective component in the reducing agent is not less than 99.0%, and the heat stability is more than 50 minutes at 95 ± 0.5.
5. The method for preparing reduced liquid indigo according to claim 1, wherein the reaction vessel is a stainless steel jacketed reaction vessel with a capacity of 5m, the built-in dispersion plate is capable of frequency modulation, the motor is connected in a three-phase five-wire system, and the working voltage is 380V.
6. The method for preparing reduced liquid indigo according to claim 5, wherein the reaction kettle is provided with a cold water cooling unit for cooling the materials inside, the cold water cooling unit can cool the materials inside the reaction kettle to 4 ℃ at the minimum, and the amount of cold water conveyed by the cold water cooling unit is 200 Kg/h.
7. The method for producing reduced liquid indigo according to claim 1, wherein in step S7, compressed air is produced by an air compression system having a compressed air production amount of 210 cc/hr, and the nitrogen gas is produced by a nitrogen production system.
8. The method for producing reduced liquid indigo according to claim 7, wherein the nitrogen production system produces nitrogen at a nitrogen production rate of 10 cubic/hour and a purity of produced nitrogen is 99.0% or more.
9. The method for preparing reduced liquid indigo according to claim 1, wherein the packaging container for separately packaging the reduced liquid indigo in step S7 is a tank or a ton drum.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010785779.8A CN111892827A (en) | 2020-08-06 | 2020-08-06 | Preparation method of reduced liquid indigo |
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| CN202010785779.8A CN111892827A (en) | 2020-08-06 | 2020-08-06 | Preparation method of reduced liquid indigo |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109504118A (en) * | 2018-09-27 | 2019-03-22 | 魏广华 | A kind of preparation of prereduction water solubility bipseudoindoxyl dye and storage method |
| CN109504117A (en) * | 2018-08-08 | 2019-03-22 | 魏广华 | A kind of prereduction water solubility bipseudoindoxyl dye and preparation method thereof |
-
2020
- 2020-08-06 CN CN202010785779.8A patent/CN111892827A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109504117A (en) * | 2018-08-08 | 2019-03-22 | 魏广华 | A kind of prereduction water solubility bipseudoindoxyl dye and preparation method thereof |
| CN109504118A (en) * | 2018-09-27 | 2019-03-22 | 魏广华 | A kind of preparation of prereduction water solubility bipseudoindoxyl dye and storage method |
Non-Patent Citations (2)
| Title |
|---|
| 张冀鄂、丁文才: "《染整使用仿色技术》", 31 August 2011, 东华大学出版社 * |
| 赵涛: "《染整工艺与原理 下册》", 31 January 2020, 中国纺织出版社 * |
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