CN104651543A - Preparation method of filling-foaming-type leather re-tanning agent - Google Patents
Preparation method of filling-foaming-type leather re-tanning agent Download PDFInfo
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- CN104651543A CN104651543A CN201310588001.8A CN201310588001A CN104651543A CN 104651543 A CN104651543 A CN 104651543A CN 201310588001 A CN201310588001 A CN 201310588001A CN 104651543 A CN104651543 A CN 104651543A
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- polyethylene glycol
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- glycol monooleate
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- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C3/00—Tanning; Compositions for tanning
- C14C3/02—Chemical tanning
- C14C3/08—Chemical tanning by organic agents
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- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
A preparation method of a filling-foaming-type leather re-tanning agent is characterized by includes following steps: (1) preparation of maleic acid polyethylene glycol monooleate: feeding polyethylene glycol-400 and oleic acid into a reactor and performing a reaction at 80-85 DEG C for 1.5-2.0 h, and adding maleic anhydride and performing the reaction with temperature maintenance for 1.0-1.5 h to obtain the maleic acid polyethylene glycol monooleate, wherein the mass ratio of the polyethylene glycol-400, the oleic acid to the maleic anhydride is 10:7:2.4; (2) preparation of the filling-foaming-type leather re-tanning agent: mixing the maleic acid polyethylene glycol monooleate, propene sulfonate, acrylamide and acrylonitrile according to a mass ratio of 12.5:1:2:0.5 to obtain a mixed monomer, adding 25-30 parts by weight of pure water to the reactor, slowly adding 16 parts by weight of the mixed monomer and 20 parts by weight of an ammonium persulfate water solution when the temperature of water is 70-75 DEG C respectively with a material feeding time being 0.5-1 h, wherein the mass fraction of the ammonium persulfate in the water solution is 0.75%, performing a thermal-insulated reaction at 80-85 DEG C for 2.0-2.5 h after material feeding finished, and finally regulating the pH value to 6.0-6.5 by a sodium hydroxide being 30% in mass fraction to obtain the re-tanning agent.
Description
Technical field
The present invention relates to a kind of preparation method of ethylene monomer copolymer type leather retanning agent, particularly a kind of preparation method of filling-foam leather composite tanning agent.
Background technology
China is that world leather is produced and the center of processing now, be a large amount of foreign exchange of national extra earning and increase millions of job opportunities every year.The leather chemicals of hundreds of kinds is needed in leather production process, wherein leather composite tanning agent has the title of " Golden Touch " in leather is produced, the retanning agent of excellent performance can change the style of leather, improve the quality scale of leather, increases added value and the economic benefit of leather significantly.Selective filling performance is good and application can be made to remove from office have the filling-foam leather composite tanning agent of feel as soft sponge to be the urgent expectation of the focus studied of people and leather-making enterprises always.The position that the select operator of retanning agent well just can reduce whole leather is poor, improves the utilization ratio of leather; Foaming sense is exactly by force soft and springiness, and its effect to improve the quality scale of leather and the value of use.At present, domestic and international leather does not also have the filling-foam leather composite tanning agent that can meet production requirement in producing.In actual production, the effect that filling-foam leather often will lean on experienced leather technology personnel to rely on the synergy of relevant weighting agent, retanning agent and fatting agent can reach more satisfactory, also makes leather processing technique and complicate.Therefore, produce in the urgent need to the exsertile filling-foam leather composite tanning agent of one at leather, the production technique of filling-foam leather is simplified.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of filling-foam leather composite tanning agent, when the retanning agent obtained according to preparation method of the present invention is applied to leather, there is application art simple, effect is remarkable, make application leather have the good and soft sponge sense of select operator, the style of leather can be improved significantly; For achieving the above object, the preparation method that the present invention adopts is:
The preparation of maleic acid polyethylene glycol monooleate: PEG-4000 and oleic acid are added reactor and react 1.5-2.0 hour when 80-85 DEG C, add MALEIC ANHYDRIDE again and continue insulation reaction 1.0-1.5 hour, obtain maleic acid polyethylene glycol monooleate, the mass ratio of said PEG-4000, oleic acid and MALEIC ANHYDRIDE is 10: 7: 2.4;
The preparation of filling-foam leather composite tanning agent: by maleic acid polyethylene glycol monooleate, Sodium allyl sulphonate, acrylamide and vinyl cyanide are mixed and made into mix monomer by the mass ratio of 12.5: 1: 2: 0.5, then the pure water that mass fraction is 25-30 part is added in the reactor, slowly adding mass parts respectively when water temperature is 70-75 DEG C is the mix monomer of 16 parts and the ammonium persulfate aqueous solution of 20 parts, ammonium persulphate massfraction 0.75% in said ammonium persulfate aqueous solution, feed time is 0.5-1.0 hour, in 80 DEG C of-85 DEG C of insulation reaction 2.0-2.5 hour after reinforced, be finally 6.0-6.5 by the sodium hydroxide solution adjust ph that massfraction is 30%, the present invention prepares filling-foam leather composite tanning agent by the copolymerization of maleic acid polyethylene glycol monooleate and Sodium allyl sulphonate, acrylamide and vinyl cyanide, by the filling of retanning agent and fatting agent and frothing function by the feature functionality base in molecular chain and side base and leather fiber be used for realize.The synthesis technique of this filling-foam leather composite tanning agent is unique, Be very effective.
Embodiment
Embodiment 1: first PEG-4000 and oleic acid are added in reactor, 1.5 hours are reacted 80 DEG C time, add MALEIC ANHYDRIDE again and continue insulation reaction 1.0 hours, obtain maleic acid polyethylene glycol monooleate, the mass ratio of PEG-4000, oleic acid and MALEIC ANHYDRIDE is 10: 7: 2.4, again by maleic acid polyethylene glycol monooleate, Sodium allyl sulphonate, acrylamide and vinyl cyanide are mixed and made into mix monomer by the mass ratio of 12.5: 1: 2: 0.5, then the pure water that mass fraction is 25 parts is added in the reactor, adding mass fraction respectively at leisure when water temperature is 70 DEG C is the mix monomer of 16 parts and the ammonium persulfate aqueous solution of 20 parts, in ammonium persulfate aqueous solution, ammonium persulphate massfraction is 0.75%, feed time is 0.5 hour, in 80 DEG C of insulation reaction 2.0 hours after reinforced, be finally 6.0 by the sodium hydroxide solution adjust ph that massfraction is 30%, embodiment 2: first PEG-4000 and oleic acid are added in reactor, 1.6 hours are reacted 83 DEG C time, add MALEIC ANHYDRIDE again and continue insulation reaction 1.2 hours, obtain maleic acid polyethylene glycol monooleate, the mass ratio of PEG-4000, oleic acid and MALEIC ANHYDRIDE is 10: 7: 2.4, again by maleic acid polyethylene glycol monooleate, Sodium allyl sulphonate, acrylamide and vinyl cyanide are mixed and made into mix monomer by the mass ratio of 12.5: 1: 2: 0.5, then the pure water that mass fraction is 29 parts is added in the reactor, adding mass fraction respectively at leisure when water temperature is 75 DEG C is the mix monomer of 16 parts and the ammonium persulfate aqueous solution of 20 parts, in ammonium persulfate aqueous solution, ammonium persulphate massfraction is 0.75%, feed time is 0.9 hour, in 82 DEG C of insulation reaction 2.5 hours after reinforced, be finally 6.1 by the sodium hydroxide solution adjust ph that massfraction is 30%, embodiment 3: first PEG-4000 and oleic acid are added in reactor, 1.9 hours are reacted 81 DEG C time, add MALEIC ANHYDRIDE again and continue insulation reaction 1.5 hours, obtain maleic acid polyethylene glycol monooleate, the mass ratio of PEG-4000, oleic acid and MALEIC ANHYDRIDE is 10: 7: 2.4, again by maleic acid polyethylene glycol monooleate, Sodium allyl sulphonate, acrylamide and vinyl cyanide are mixed and made into mix monomer by the mass ratio of 12.5: 1: 2: 0.5, then the pure water that mass fraction is 27 parts is added in the reactor, adding mass fraction respectively at leisure when water temperature is 72 DEG C is the mix monomer of 16 parts and the ammonium persulfate aqueous solution of 20 parts, in ammonium persulfate aqueous solution, ammonium persulphate massfraction is 0.75%, feed time is 0.6 hour, in 85 DEG C of insulation reaction 2.1 hours after reinforced, be finally 6.5 by the sodium hydroxide solution adjust ph that massfraction is 30%, embodiment 4: first PEG-4000 and oleic acid are added in reactor, 1.7 hours are reacted 84 DEG C time, add MALEIC ANHYDRIDE again and continue insulation reaction 1.1 hours, obtain maleic acid polyethylene glycol monooleate, the mass ratio of PEG-4000, oleic acid and MALEIC ANHYDRIDE is 10: 7: 2.4, again by maleic acid polyethylene glycol monooleate, Sodium allyl sulphonate, acrylamide and vinyl cyanide are mixed and made into mix monomer by the mass ratio of 12.5: 1: 2: 0.5, then the pure water that mass fraction is 26 parts is added in the reactor, adding mass fraction respectively at leisure when water temperature is 74 DEG C is the mix monomer of 16 parts and the ammonium persulfate aqueous solution of 20 parts, in ammonium persulfate aqueous solution, ammonium persulphate massfraction is 0.75%, feed time is 0.7 hour, in 81 DEG C of insulation reaction 2.3 hours after reinforced, be finally 6.3 by the sodium hydroxide solution adjust ph that massfraction is 30%.
Claims (3)
1. the preparation method of a filling-foam leather composite tanning agent, it is characterized in that: the preparation of (1) maleic acid polyethylene glycol monooleate: PEG-4000 and oleic acid are added reactor and react 1.5-2.0 hour when 80-85 DEG C, add MALEIC ANHYDRIDE again and continue insulation reaction 1.0-1.5 hour, obtain maleic acid polyethylene glycol monooleate, the mass ratio of said PEG-4000, oleic acid and MALEIC ANHYDRIDE is 10: 7: 2.4, 2) preparation of filling-foam leather composite tanning agent: by maleic acid polyethylene glycol monooleate, Sodium allyl sulphonate, acrylamide and vinyl cyanide are mixed and made into mix monomer by the mass ratio of 12.5: 1: 2: 0.5, then the pure water that mass fraction is 25-30 part is added in the reactor, slowly adding mass fraction respectively when water temperature is 70-75 DEG C is the mix monomer of 16 parts and the ammonium persulfate aqueous solution of 20 parts, in said ammonium persulfate aqueous solution, ammonium persulphate massfraction is 0.75%, feed time is 0.5-1.0 hour, in 80 DEG C of-85 DEG C of insulation reaction 2.0-2.5 hour after reinforced, be finally 6.0-6.5 by the sodium hydroxide solution adjust ph that massfraction is 30%.
2. the preparation method of filling-foam leather composite tanning agent according to claim 1, it is characterized in that: first PEG-4000 and oleic acid are added in reactor, 1.5 hours are reacted 80 DEG C time, add MALEIC ANHYDRIDE again and continue insulation reaction 1.0 hours, obtain maleic acid polyethylene glycol monooleate, the mass ratio of PEG-4000, oleic acid and MALEIC ANHYDRIDE is 10: 7: 2.4, again by maleic acid polyethylene glycol monooleate, Sodium allyl sulphonate, acrylamide and vinyl cyanide are mixed and made into mix monomer by the mass ratio of 12.5: 1: 2: 0.5, then the pure water that mass fraction is 25 parts is added in the reactor, adding mass fraction respectively at leisure when water temperature is 70 DEG C is the mix monomer of 16 parts and the ammonium persulfate aqueous solution of 20 parts, in ammonium persulfate aqueous solution, ammonium persulphate massfraction is 0.75%, feed time is 0.5 hour, in 80 DEG C of insulation reaction 2.0 hours after reinforced, be finally 6.0 by the sodium hydroxide solution adjust ph that massfraction is 30%.
3. filling-foam leather composite tanning agent preparation method according to claim 1, it is characterized in that: first PEG-4000 and oleic acid are added in reactor, 1.6 hours are reacted 83 DEG C time, add MALEIC ANHYDRIDE again and continue insulation reaction 1.2 hours, obtain maleic acid polyethylene glycol monooleate, the mass ratio of PEG-4000, oleic acid and MALEIC ANHYDRIDE is 10: 7: 2.4, again by maleic acid polyethylene glycol monooleate, Sodium allyl sulphonate, acrylamide and vinyl cyanide are mixed and made into mix monomer by the mass ratio of 12.5: 1: 2: 0.5, then the pure water that mass fraction is 29 parts is added in the reactor, adding mass fraction respectively at leisure when water temperature is 75 DEG C is the mix monomer of 16 parts and the ammonium persulfate aqueous solution of 20 parts, in ammonium persulfate aqueous solution, ammonium persulphate massfraction is 0.75%, feed time is 0.9 hour, in 82 DEG C of insulation reaction 2.5 hours after reinforced, be finally 6.1 by the sodium hydroxide solution adjust ph that massfraction is 30%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310588001.8A CN104651543A (en) | 2013-11-21 | 2013-11-21 | Preparation method of filling-foaming-type leather re-tanning agent |
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| CN201310588001.8A CN104651543A (en) | 2013-11-21 | 2013-11-21 | Preparation method of filling-foaming-type leather re-tanning agent |
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| CN201310588001.8A Pending CN104651543A (en) | 2013-11-21 | 2013-11-21 | Preparation method of filling-foaming-type leather re-tanning agent |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029343A (en) * | 2007-01-25 | 2007-09-05 | 陕西科技大学 | Production of filling-foam leather composite tanning agent |
| CN101886093A (en) * | 2010-06-22 | 2010-11-17 | 陕西科技大学 | Preparation method of phenol leather synthetic tanning agent through HRP (Horse Radish Peroxidase) catalytic synthesis |
| CN102747173A (en) * | 2012-07-02 | 2012-10-24 | 陕西科技大学 | Preparation method of aluminum-oxidized starch complex tanning agent |
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- 2013-11-21 CN CN201310588001.8A patent/CN104651543A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029343A (en) * | 2007-01-25 | 2007-09-05 | 陕西科技大学 | Production of filling-foam leather composite tanning agent |
| CN101886093A (en) * | 2010-06-22 | 2010-11-17 | 陕西科技大学 | Preparation method of phenol leather synthetic tanning agent through HRP (Horse Radish Peroxidase) catalytic synthesis |
| CN102747173A (en) * | 2012-07-02 | 2012-10-24 | 陕西科技大学 | Preparation method of aluminum-oxidized starch complex tanning agent |
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Application publication date: 20150527 |