CN1311032C - New-type leather black and its production process - Google Patents
New-type leather black and its production process Download PDFInfo
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- CN1311032C CN1311032C CNB2004100645807A CN200410064580A CN1311032C CN 1311032 C CN1311032 C CN 1311032C CN B2004100645807 A CNB2004100645807 A CN B2004100645807A CN 200410064580 A CN200410064580 A CN 200410064580A CN 1311032 C CN1311032 C CN 1311032C
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Abstract
The present invention relates to new leather black which comprises sulfur black and a modifying agent as raw materials, wherein the modifying agent is composed of chloroactic acid, sodium metabisulfite, sodium sulfide and sodium hydroxide. A production process of the new leather black comprises a preparing process of a sulfur black solution, a preparing process of a modifying agent solution, a mixing process of the sulfur black solution and the modifying agent solution, and a baking and pulverizing process. The sulfur black is reduced to a leuco body thereof by the present invention, and then a hydrophilic radical-carboxylic acid group and a sulfonic group are orderly led in the molecular structure of the sulfur black so that the solubility of the sulfur black is further improved; the leading-in proportion of the carboxylic acid group and the sulfonic group can be controlled in the process so that the present invention can achieve different quality requirements, and then leather block containing the sulfonic group as well as carboxylic acid is obtained. Compared with the leather black produced by the prior art, the blackness of the new leather black of the present invention is greatly enhanced; because the carboxylic acid group and the sulfonic group are simultaneously led in the production process of the leather black, the present invention enhances the rubbing firmness of the leather black and meet the different requirements of people.
Description
Technical field
The present invention relates to a kind of leather coloring dedicated dye and production technique thereof, be specially New-type leather black and production technique thereof.
Background technology
At present, in the production technique of leather black, used raw material comprises sulphur black and properties-correcting agent, has plenty of in the sulphur black molecular structure and introduces hydrophilic radical-sulfonic group, make it water-solublely obtain containing sulfonic solubilised sulphur black, properties-correcting agent comprises Sodium Pyrosulfite, caustic soda; Have plenty of sulphur black is reduced into its leuco compound, introduce hydrophilic radical-carboxylic acid group again in its molecular structure, make its water-soluble solubilised sulphur black that obtains containing the carboxylic acid group, properties-correcting agent comprises Mono Chloro Acetic Acid, Sodium Sulphide, caustic soda; These two kinds of production methods substantially all comprise mixing process, oven dry, the crushing process of configuration, sulphur black solution and modifier solution of configuration, the modifier solution of sulphur black solution, yet, though the leather black that these production methods are produced is each has something to recommend him on every performance, but it is, also very undesirable at aspects such as pitch black degree and friction fastness.
Summary of the invention
The present invention provides a kind of New-type leather black, and its production method is provided for performances such as the pitch black degree that improves existing leather black and the fastness that rubs.
Technical scheme of the present invention realizes in the following way: a kind of New-type leather black, its raw material comprises sulphur black and properties-correcting agent, properties-correcting agent is made up of Mono Chloro Acetic Acid, Sodium Pyrosulfite, Sodium Sulphide, caustic soda, and the weight ratio of each component is: sulphur black: Mono Chloro Acetic Acid: Sodium Pyrosulfite: Sodium Sulphide: caustic soda=1: 4.5-5.5: 2-2.5: 2.3: 9.
Its production technique comprises mixing process, oven dry, the crushing process of configuration, sulphur black solution and modifier solution of configuration, the modifier solution of sulphur black solution, wherein, the layoutprocedure of sulphur black solution is as follows: add suitable quantity of water in reactor, and stir, sulphur black is added in the entry, is warming up to 85 ℃--95 ℃, add Sodium Sulphide, proportion is adjusted into 1-1.4l/g, is incubated 5-6h then; The layoutprocedure of modifier solution comprises the configuration of preparation of sodium chloroacetate liquid and metabisulfite solution, wherein the configuration of metabisulfite solution is identical with the collocation method in the technology of existing production leather black, only need its concentration adjustment to 25%, the process for preparation of sodium chloroacetate solution is as follows: add caustic soda in stirring condition downhill reaction still, then ice cube is added in the reactor, make liquid temperature drop to 0 ℃, Mono Chloro Acetic Acid is added in the reactor again and react, the reaction times is 25min-35min; The mixing process of sulphur black solution and modifier solution comprises carboxylation mixing and sulfonation mixing process, carboxylation mixing process is as follows: the sulphur black solution that configures is added in the sodium chloroacetate solution mix, make the temperature of mixed solution rise to 60 ℃--65 ℃, be incubated 2-2.5h then, promptly made carboxylation liquid; Sulfonation mixing process is as follows: the sodium metabisulfite solution of slow dropping 25% in carboxylation liquid, after dropwising, insulation 35--45min is dried then, is pulverized, and promptly has been made into finished product.The carboxylic acid group can decide according to different needs with sulfonic introducing ratio.
The present invention is reduced into its leuco compound with sulphur black, in its molecular structure, successively introduce hydrophilic radical-carboxylic acid group and sulfonic group again, further improved its solvability, and can in technological process, control carboxylic acid group and sulfonic introducing ratio, thereby can reach different specification of quality, not only contained sulfonic group but also contained carboxylic acid group's leather black.Compare, differentiate and judge by the leather black of with the naked eye producing with prior art, the pitch black degree of New-type leather black of the present invention improves greatly, its the friction fastness raising can illustrate by following table (GB of fastness index is: the dry friction fastness--4, the wet-milling rubbing fastness--3):
As can be seen from the above table, because the present invention has introduced carboxylic acid group and sulfonic group simultaneously in the production technique of leather black, so, compare with the leather black that prior art is produced, improved the friction fastness of leather black, greatly satisfied people's different demands.
Embodiment
Embodiment 1: a kind of New-type leather black, its raw material comprises sulphur black and properties-correcting agent, properties-correcting agent is made up of Mono Chloro Acetic Acid, Sodium Pyrosulfite, Sodium Sulphide, caustic soda, the weight ratio of each component (sulphur black: Mono Chloro Acetic Acid: Sodium Pyrosulfite: Sodium Sulphide: caustic soda) be 1: 4.5: 2: 2.3: 9.
Its production technique comprises mixing process, oven dry, the crushing process of configuration, sulphur black solution and modifier solution of configuration, the modifier solution of sulphur black solution, wherein, the layoutprocedure of sulphur black solution is as follows: add suitable quantity of water in reactor, and stir, sulphur black is added in the entry, be warming up to 85 ℃, add Sodium Sulphide, solution proportion is adjusted to 1l/g, is incubated 5h then; The layoutprocedure of modifier solution comprises the configuration of preparation of sodium chloroacetate liquid and metabisulfite solution, wherein the configuration of metabisulfite solution is identical with the collocation method in the technology of existing production leather black, only need its concentration adjustment to 25%, the process for preparation of sodium chloroacetate solution is as follows: add caustic soda in stirring condition downhill reaction still, then ice cube is added in the reactor, make liquid temperature drop to 0 ℃, Mono Chloro Acetic Acid is added in the reactor again and react, the reaction times is 25min; The mixing process of sulphur black solution and modifier solution comprises carboxylation mixing and sulfonation mixing process, carboxylation mixing process is as follows: the sulphur black solution that configures is added in the sodium chloroacetate solution mix, make the temperature of mixed solution rise to 60 ℃, be incubated 2h then, promptly made carboxylation liquid; Sulfonation mixing process is as follows: the sodium metabisulfite solution of slow dropping 25% in carboxylation liquid, after dropwising, insulation 35min is dried then, is pulverized, and promptly has been made into finished product.
Embodiment 2: a kind of New-type leather black, its raw material comprises sulphur black and properties-correcting agent, properties-correcting agent is made up of Mono Chloro Acetic Acid, Sodium Pyrosulfite, Sodium Sulphide, caustic soda, the weight ratio of each component (sulphur black: Mono Chloro Acetic Acid: Sodium Pyrosulfite: Sodium Sulphide: caustic soda) be 1: 5.5: 2.5: 2.3: 9.
Its production technique comprises mixing process, oven dry, the crushing process of configuration, sulphur black solution and modifier solution of configuration, the modifier solution of sulphur black solution, wherein, the layoutprocedure of sulphur black solution is as follows: add suitable quantity of water in reactor, and stir, sulphur black is added in the entry, be warming up to 95 ℃, add Sodium Sulphide, solution proportion is adjusted to 1.4l/g, is incubated 6h then; The layoutprocedure of modifier solution comprises the configuration of preparation of sodium chloroacetate liquid and metabisulfite solution, wherein the configuration of metabisulfite solution is identical with the collocation method in the technology of existing production leather black, only need its concentration adjustment to 25%, the process for preparation of sodium chloroacetate solution is as follows: add caustic soda in stirring condition downhill reaction still, then ice cube is added in the reactor, make liquid temperature drop to 0 ℃, Mono Chloro Acetic Acid is added in the reactor again and react, the reaction times is 35min; The mixing process of sulphur black solution and modifier solution comprises carboxylation mixing and sulfonation mixing process, carboxylation mixing process is as follows: the sulphur black solution that configures is added in the sodium chloroacetate solution mix, make the temperature of mixed solution rise to 65 ℃, be incubated 2.5h then, promptly made carboxylation liquid; Sulfonation mixing process is as follows: the sodium metabisulfite solution of slow dropping 25% in carboxylation liquid, after dropwising, insulation 45min is dried then, is pulverized, and promptly has been made into finished product.
Embodiment 3: a kind of New-type leather black, its raw material comprises sulphur black and properties-correcting agent, properties-correcting agent is made up of Mono Chloro Acetic Acid, Sodium Pyrosulfite, Sodium Sulphide, caustic soda, the weight ratio of each component (sulphur black: Mono Chloro Acetic Acid: Sodium Pyrosulfite: Sodium Sulphide: caustic soda) be 1: 5: 2.25: 2.3: 9.
Its production technique comprises mixing process, oven dry, the crushing process of configuration, sulphur black solution and modifier solution of configuration, the modifier solution of sulphur black solution, wherein, the layoutprocedure of sulphur black solution is as follows: add suitable quantity of water in reactor, and stir, sulphur black is added in the entry, be warming up to 90 ℃, add Sodium Sulphide, proportion is adjusted into 1.2l/g, is incubated 5.5h then; The layoutprocedure of modifier solution comprises the configuration of preparation of sodium chloroacetate liquid and metabisulfite solution, wherein the configuration of metabisulfite solution is identical with the collocation method in the technology of existing production leather black, only need its concentration adjustment to 25%, the process for preparation of sodium chloroacetate solution is as follows: add caustic soda in stirring condition downhill reaction still, then ice cube is added in the reactor, make liquid temperature drop to 0 ℃, Mono Chloro Acetic Acid is added in the reactor again and react, the reaction times is 30min; The mixing process of sulphur black solution and modifier solution comprises carboxylation mixing and sulfonation mixing process, carboxylation mixing process is as follows: the sulphur black solution that configures is added in the sodium chloroacetate solution mix, make the temperature of mixed solution rise to 62.5 ℃, be incubated 2.25h then, promptly made carboxylation liquid; Sulfonation mixing process is as follows: the sodium metabisulfite solution of slow dropping 25% in carboxylation liquid, after dropwising, insulation 40min is dried then, is pulverized, and promptly has been made into finished product.
Claims (2)
1, a kind of New-type leather black, its raw material comprises sulphur black and properties-correcting agent, it is characterized in that: properties-correcting agent is made up of Mono Chloro Acetic Acid, Sodium Pyrosulfite, Sodium Sulphide, caustic soda, and the weight ratio of each component is: sulphur black: Mono Chloro Acetic Acid: Sodium Pyrosulfite: Sodium Sulphide: caustic soda=1: 4.5-5.5: 2-2.5: 2.3: 9.
2, the production technique of New-type leather black according to claim 1, mixing process, oven dry, the crushing process of configuration, sulphur black solution and modifier solution that comprises configuration, the modifier solution of sulphur black solution, it is characterized in that: wherein, the layoutprocedure of sulphur black solution is as follows: add suitable quantity of water in reactor, and stir, sulphur black is added in the entry, be warming up to 85 ℃--95 ℃, add Sodium Sulphide, proportion is adjusted into 1-1.4l/g, is incubated 5-6h then; The layoutprocedure of modifier solution comprises the configuration of preparation of sodium chloroacetate liquid and metabisulfite solution, wherein the configuration of metabisulfite solution is identical with the collocation method in the technology of existing production leather black, only need its concentration adjustment to 25%, the process for preparation of sodium chloroacetate solution is as follows: add caustic soda in stirring condition downhill reaction still, then ice cube is added in the reactor, make liquid temperature drop to 0 ℃, Mono Chloro Acetic Acid is added in the reactor again and react, the reaction times is 25min-35min; The mixing process of sulphur black solution and modifier solution comprises carboxylation mixing and sulfonation mixing process, carboxylation mixing process is as follows: the sulphur black solution that configures is added in the sodium chloroacetate solution mix, make the temperature of mixed solution rise to 60 ℃--65 ℃, be incubated 2-2.5h then, promptly made carboxylation liquid; Sulfonation mixing process is as follows: the sodium metabisulfite solution of slow dropping 25% in carboxylation liquid, after dropwising, insulation 35--45min is dried then, is pulverized, and promptly has been made into finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100645807A CN1311032C (en) | 2004-12-03 | 2004-12-03 | New-type leather black and its production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100645807A CN1311032C (en) | 2004-12-03 | 2004-12-03 | New-type leather black and its production process |
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| Publication Number | Publication Date |
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| CN1637205A CN1637205A (en) | 2005-07-13 |
| CN1311032C true CN1311032C (en) | 2007-04-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2004100645807A Expired - Fee Related CN1311032C (en) | 2004-12-03 | 2004-12-03 | New-type leather black and its production process |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103627209A (en) * | 2013-10-22 | 2014-03-12 | 大连市旅顺口区江西化工工业总公司 | Preparation method of polycarboxy water-soluble sulfur black |
| CN105331144B (en) * | 2015-11-02 | 2017-03-22 | 深圳市国华光电科技有限公司 | Pure black dye and preparation method thereof and electrowetting display printing ink |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53134825A (en) * | 1977-04-28 | 1978-11-24 | Mitsubishi Chem Ind Ltd | Dye composition |
| CN1072697A (en) * | 1991-10-11 | 1993-06-02 | 山道士有限公司 | Sulfur dye composition and production thereof |
| CN1426441A (en) * | 2000-04-20 | 2003-06-25 | 宝洁公司 | Sulfur dye protection systems and compositions and methods employing same |
-
2004
- 2004-12-03 CN CNB2004100645807A patent/CN1311032C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53134825A (en) * | 1977-04-28 | 1978-11-24 | Mitsubishi Chem Ind Ltd | Dye composition |
| CN1072697A (en) * | 1991-10-11 | 1993-06-02 | 山道士有限公司 | Sulfur dye composition and production thereof |
| CN1426441A (en) * | 2000-04-20 | 2003-06-25 | 宝洁公司 | Sulfur dye protection systems and compositions and methods employing same |
Non-Patent Citations (1)
| Title |
|---|
| 新型水溶性硫化黑在棉织物上的应用 王梅 杨锦宗 张勇，纺织学报，第22卷第3期 2001 * |
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| CN1637205A (en) | 2005-07-13 |
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