CN106518955B - A method of hair depilation recycling ox hair, which is protected, with process hides prepares process hides protein filling - Google Patents
A method of hair depilation recycling ox hair, which is protected, with process hides prepares process hides protein filling Download PDFInfo
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- CN106518955B CN106518955B CN201610983143.8A CN201610983143A CN106518955B CN 106518955 B CN106518955 B CN 106518955B CN 201610983143 A CN201610983143 A CN 201610983143A CN 106518955 B CN106518955 B CN 106518955B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/34—Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/12—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length by hydrolysis, i.e. solvolysis in general
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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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Abstract
The invention discloses a kind of methods for protecting hair depilation recycling ox hair preparation process hides protein filling with process hides, with alkaline process synergetic hydrolysis ox hair, to filter its main feature is that protecting hair depilation recycling ox hair as raw material using process hides and collect filtrate；Filter residue is hydrolyzed under high-temperature and high-pressure conditions again with a small amount of highly basic, is filtered and is collected filtrate；The filtrate collected twice is mixed, obtains solid-state protein filler up to liquid protein filling, or after drying with after inorganic acid tune pH；And by filter residue high-temperature roasting, obtained powder is back in ox hair basic hydrolysis.The present invention quickly filters after being able to achieve ox hair hydrolysis, and obtained liquid or solid-state protein filler color is light, and ox hair percent hydrolysis is high, and does not generate solid waste, is a kind of method of easy to operate, economical and practical industrialized production protein filling.
Description
Technical field
The invention belongs to prepare the method for protolysate, in particular to a kind of to protect hair depilation recycling ox hair with process hides be former
The method of material preparation process hides protein filling.
Background technique
The pollution caused by waste water of mao epilation is ruined in order to reduce, leather-making enterprises, which are just widelyd popularize to apply, keeps ox hair completeer
The whole hair saving process to fall off.Thus obtained recycling ox hair enormous amount and be rich in keratin, resource can be subject to after recycling
Change and utilizes.In leather industry, recycling ox hair can be hydrolyzed to the suitable protolysate of molecular weight distribution and be filled out to prepare albumen
Material is used for process hides retanning filling work procedure, and the leather with good hand and sanitation performance is made.This is not only resource utilization ox
The effective way of hair, and meet the demand for development of circular economy.Currently, the method for hydrolysis ox hair has acid-hydrolysis method, basic hydrolysis
Method, enzyme hydrolysis method, hydrogen peroxide Hydrolyze method, alkali-enzyme synergetic hydrolysis method etc..Stable structure in alkali hydrolysis method energy rapid damage ox hair
Cystine linkage interrupts peptide bond and sat linkage, dissolves hair completely, while its is easy to operate, and equipment requirement is low, is the extensive water of industrialization
Solve the prefered method of ox hair.
In the prior art, Chinese patent CN101260140 is " a kind of to prepare process hides protein filling by raw material of animal wool
Method " disclose it is a kind of first with inorganic acid and reducing agent dipping pretreatment, after the ox hair hydrolysis side that is hydrolyzed with alkali compounds
Method.This method is the problem is that gained protein filling color is deep, for seriously affecting the color of leather after retanning filling work procedure
And sense organ, strongly limit its application in process hides.The reason of leading to the problem of this is to contain a large amount of pigments in alkaline hydrolyzate
And the impurity such as ox hair are not hydrolyzed, but since its viscosity is big, it is in starchiness, can not be efficiently separated, can only be directly concentrated dry
It is used after dry.Chinese patent CN104523549A " a method of uvioresistant moisturizer is prepared using ox hair " disclose one kind
First use inorganic acid and alkali compounds dipping pretreatment, after with alkali compounds hydrolyze ox hair method for hydrolysis, obtained buck
Solution liquid only could separate protein liquid with solid waste through high speed centrifugation, and supernatant is equally rich in pigment, and color is deeper.
(Pu Jianmin, Mao Pei, Shen Xiaojun wait to protect the research leather science and work of hair depilation recycling ox hair basic hydrolysis technique to document
Journey, 2014,24 (3): 52-58.) it reports and a kind of first uses NaHSO3Pretreatment, after with NaOH hydrolyze ox hair hydrolysis side
Method, the problem is that the soft easily-deformable solid impurity of matter will form knot in sticky hydrolyzate during cold filtration
The easily compressed fine and close filter cake of structure, suspended particulates therein can block filtration channel, cause to be difficult to filter, while pigment remains in
In hydrolyzate, keep hydrolysate color still relatively deep.In addition, although ox hair all have passed through pretreatment and buck in these above-mentioned methods
Two-step reaction is solved, but it is useless still to generate more solid 90% hereinafter, even if being able to carry out separation after basic hydrolysis for its percent hydrolysis
Gurry.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of use for disadvantage existing in the prior art or deficiency
It is the method that raw material prepares process hides protein filling that hair depilation recycling ox hair is protected in process hides, its main feature is that being capable of quick mistake after basic hydrolysis
Simultaneously efficient decolorizing is filtered, obtained liquid or solid-state protein filler color are light, and ox hair percent hydrolysis is high, and does not generate solid waste.
A kind of method for protecting hair depilation recycling ox hair preparation process hides protein filling with process hides provided by the invention, this method
Processing step and condition it is as follows, by weight are as follows:
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 6-20 parts of highly basic, 4-10 parts of alkalinity is added
Oxide, 0.5-2 parts of sodium silicoaluminates, 500-1000 parts of water react 3-10h at 70-90 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 0.5-2 parts of highly basic, 50-100 parts of water, in pressure 0.2- is added
0.8MPa reacts 1-5h at 130-190 DEG C of temperature, filters and collect filtrate；
(3) filter residue of step (2) is roasted into 1-4h at 500-800 DEG C of temperature, obtained powder is back in step (1)
Instead of basic anhydride and sodium silicoaluminate；
(4) filtrate that step (1) and (2) are collected is mixed, using inorganic acid tune pH to 5.5-7.5, obtains liquid process hides
With protein filling, or will liquid process hides with protein filling it is dry after obtain solid-state process hides protein filling.
The alkali compounds is NaOH, Ca (OH)2At least one of with KOH.
The basic anhydride are MgO, CaO and Al2O3At least one of.
The inorganic acid is at least one of hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid.
The present invention can be realized alkaline hydrolyzate filtering and the principle of decoloration is, the filter process after ox hair basic hydrolysis
In, the basic anhydride or sodium silicoaluminate of addition help because quality is hard and in irregular shape and to form loose, multi-pore channel, can not
The filter cake of compression increases flow channel, reduces flow resistance, promotes ox hair hydrolysed mix solid-liquid quick separating；Meanwhile it is selected
Surface is in strong electropositive to the basic anhydride or sodium silicoaluminate selected at reaction conditions, and it is smaller can to adsorb electronegative partial size
Pigment and suspended particulate, the coloration of hydrolyzate can be reduced to a certain extent.Through the invention further study show that,
A certain amount of sodium silicoaluminate is added while basic anhydride are added, under the synergistic effect of the two, ox hair hydrolysed mix is not
Only can quick separating, it is often more important that can efficient decolorizing, significantly reduce the coloration of ox hair hydrolyzate, finally obtained liquid or
Solid-state protein filler color is light.Then, basic anhydride and sodium silicoaluminate enter filter residue, and the first step can be back to after being fired
In basic hydrolysis.
In addition, the inventors have found that, ox hair is in depilation liming process by the strong work of the grey materials such as alkali and sulfide
With scale layer, which has been destroyed, even to be peeled off.In ox hair hydrolytic process, cortex can be directly acted on by being directly added into highly basic
Layer.For the pretreated ox hair of distinct methods compared with not preprocessed ox hair, basic hydrolysis rate is essentially identical, and the face of hydrolysate
Color, property are similar.Therefore, ox hair need not be pre-processed before basic hydrolysis.
Compared with the prior art, the present invention has the following beneficial effects:
(1) present invention protects hair depilation recycling ox hair using highly basic, basic anhydride and sodium silicoaluminate synergetic hydrolysis process hides, with
Existing ox hair basic hydrolysis technology is compared, and has not only been able to achieve ox hair hydrolyzate and the quick of solid slag is separated by filtration, but also can efficient absorption
The pigment in ox hair hydrolyzate is removed, the coloration of hydrolyzate is significantly reduced, ensure that protein filling has in process hides retanning filling
There is excellent application effect.
(2) present invention makes ox hair percent hydrolysis reach 95% or more, with existing ox hair basic hydrolysis technology by hydrolyzing twice
It compares, significantly improves the utilization rate to keratin resource in ox hair, while further through reasonable setting hydrolysising condition, Effective Regulation
The range of molecular weight distributions of ox hair hydrolysate makes protein filling have excellent retanning filling effect.
(3) gained powder is back in basic hydrolysis by roasting remaining filter residue and replaces basic anhydride and silicon by the present invention
Sodium aluminate equally has the effect of significant drainage and decoloration.Compared with existing ox hair basic hydrolysis technology, entire method is not produced
Raw solid waste, realizes resource circulation utilization.
Specific embodiment
The present invention is specifically described below by example, it is necessary to which indicated herein is that the present embodiment is served only for this
Invention further illustrates, should not be understood as limiting the scope of the invention, the person skilled in the art in the field can basis
The content of aforementioned present invention makes some nonessential modifications and adaptations.
Embodiment 1
(1) hairs depilation recycling ox hairs are protected in 100 parts of process hides to be placed in reactor, is added 16 parts of NaOH, 4 parts of MgO, 1.5 parts
Sodium silicoaluminate, 800 parts of water react 10h at 90 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 2 parts of KOH, 100 parts of water, in pressure 0.2MPa, temperature is added
5h is reacted at 130 DEG C, filter and collects filtrate；
(3) filter residue of step (2) is roasted into 4h at 500 DEG C of temperature, obtained powder is back in step (1) and replaces
MgO and sodium silicoaluminate；
(4) filtrate that step (1) and (2) are collected is mixed, using hydrochloric acid tune pH to 6, obtains liquid process hides and filled out with albumen
Material, or solid-state process hides protein filling will be obtained after liquid process hides protein filling drying.
In this step, the coloration value of chromatism (the results are shown in Table 1) of the mixed filtrate of step (1) and (2) collection is determined.
Comparative example 1:
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 16 parts of NaOH, 800 parts of water, in temperature is added
10h is reacted at 90 DEG C of degree, is centrifuged and collects supernatant；
(2) sediment of step (1) is placed in reactor, 2 parts of KOH, 100 parts of water, in pressure 0.2MPa, temperature is added
5h is reacted at 130 DEG C, be centrifuged and collects supernatant；
(3) supernatant that step (1) and (2) are collected is mixed.
In this step, the coloration value of chromatism (the results are shown in Table 1) of the mixing supernatant of step (1) and (2) collection is determined.
Comparative example 2:
(1) hairs depilation recycling ox hairs are protected in 100 parts of process hides to be placed in reactor, is added 16 parts of NaOH, 4 parts of MgO, 800 parts
Water reacts 10h at 90 DEG C of temperature, filters and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 2 parts of KOH, 100 parts of water, in pressure 0.2MPa, temperature is added
5h is reacted at 130 DEG C, filter and collects filtrate；
(3) filtrate that step (1) and (2) are collected is mixed.
In this step, the coloration value of chromatism (the results are shown in Table 1) of the mixed filtrate of step (1) and (2) collection is determined.
Comparative example 3:
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 16 parts of NaOH, 1.5 parts of aluminosilicates is added
Sodium, 800 parts of water react 10h at 90 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 2 parts of KOH, 100 parts of water, in pressure 0.2MPa, temperature is added
5h is reacted at 130 DEG C, filter and collects filtrate；
(3) filtrate that step (1) and (2) are collected is mixed.
In this step, the coloration value of chromatism (the results are shown in Table 1) of the mixed filtrate of step (1) and (2) collection is determined.
Coloration color difference values determination method:
Mixed filtrate/the supernatant for taking 4 mL embodiments 1, comparative example 1, comparative example 2 and comparative example 3 respectively, is diluted to 20
mL.Above-mentioned 4 groups of L, a, b value is measured with spectrophotometric color measurement instrument, with comparative example 1 as a control group (because its color is most deep), is counted respectively
Calculate Δ L, Δ a, Δ b and Δ E(, refer to total color difference).Δ E is bigger, illustrates hydrolyzate and control group
More shallow compared to color, decolorizing effect is better.
1 coloration value of chromatism measurement result of table
。
As known from Table 1, the total color difference Δ E of 1 filtrate of embodiment is noticeably greater than comparative example 1, hence it is evident that better than comparative example 2 and comparison
Example 3.Thus illustrate, in the present invention, basic anhydride and sodium silicoaluminate have excellent collaboration decolorization, hydrolyzate face
Color is most shallow.Therefore, the present invention protects hair depilation recycling ox using highly basic, basic anhydride and sodium silicoaluminate synergetic hydrolysis process hides
Hair, energy efficient absorption remove the pigment in ox hair hydrolyzate, significantly reduce the coloration of hydrolyzate.
Embodiment 2
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 6 parts of KOH, 8 parts of CaO, 1 part of sial is added
Sour sodium, 1000 parts of water, reacts 8h under temperature 70 C, filters and collects filtrate；
(2) filter residue of step (1) is placed in reactor, 0.5 part of NaOH, 0.5 part of Ca (OH) is added2, 0.5 part of KOH, 50
Part water, reacts 2h at pressure 0.8MPa, 190 DEG C of temperature, filters and collect filtrate；
(3) filter residue of step (2) is roasted into 1h at 800 DEG C of temperature, obtained powder is back in step (1) and replaces
CaO and sodium silicoaluminate；
(4) filtrate that step (1) and (2) are collected is mixed, using sulfuric acid tune pH to 7.5, obtains liquid process hides albumen
Filler, or it is dried to obtain process hides solid-state protein filler.
Embodiment 3
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 20 parts of Ca (OH) is added2, 2 parts of CaO, 2 parts
Al2O3, 2 parts of MgO, 1 part of sodium silicoaluminate, 700 parts of water react 6h at 87 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 0.5 part of NaOH, 80 parts of water, in pressure 0.6MPa, temperature is added
3h is reacted at 170 DEG C, filter and collects filtrate；
(3) filter residue of step (2) is roasted into 3h at 700 DEG C of temperature, obtained powder is back in step (1) and replaces
CaO、Al2O3, MgO and sodium silicoaluminate；
(4) filtrate that step (1) and (2) are collected is mixed, using nitric acid tune pH to 6, obtains liquid process hides and filled out with albumen
Material, or it is dried to obtain solid-state process hides protein filling.
Embodiment 4
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 8 parts of Ca (OH) is added2, 8 parts of NaOH, 4 parts
MgO, 6 parts of CaO, 0.5 part of sodium silicoaluminate, 500 parts of water react 3h at 90 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 0.5 part of KOH, 0.5 part of NaOH, 80 parts of water, in pressure is added
0.5MPa reacts 3h at 150 DEG C of temperature, filters and collect filtrate；
(3) filter residue of step (2) is roasted into 2h at 800 DEG C of temperature, obtained powder is back in step (1) and replaces
MgO, CaO and sodium silicoaluminate；
(4) filtrate collected in step (1) and (2) is mixed, using nitric acid and phosphoric acid tune pH to 5.5, obtains liquid system
Leather protein filling, or it is dried to obtain solid-state process hides protein filling.
Embodiment 5
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 6 parts of Ca (OH) is added2, 10 parts of KOH, 3 parts
MgO, 3 parts of Al2O3, 1 part of sodium silicoaluminate, 600 parts of water react 10h at 80 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 0.5 part of NaOH, 1.5 parts of Ca (OH) is added2, 70 parts of water are pressing
Strong 0.7MPa reacts 3h at 150 DEG C of temperature, filters and collect filtrate；
(3) filter residue of step (2) is roasted into 1h at 800 DEG C of temperature, obtained powder is back in step (1) and replaces
MgO、Al2O3And sodium silicoaluminate；
(4) filtrate that step (1) and (2) are collected is mixed, using nitric acid and hydrochloric acid tune pH to 7, obtains liquid process hides use
Protein filling, or it is dried to obtain solid-state process hides protein filling.
Embodiment 6
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 6 parts of NaOH, 6 parts of KOH, 3 parts of CaO is added,
3 parts of Al2O3, 1.5 parts of sodium silicoaluminates, 600 parts of water react 6 h at 85 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 0.5 part of KOH, 1.5 parts of Ca (OH) is added2, 100 parts of water are pressing
Strong 0.6MPa reacts 2h at 170 DEG C of temperature, filters and collect filtrate；
(3) filter residue of step (2) is roasted into 4h at 600 DEG C of temperature, obtained powder is back in step (1) and replaces
CaO、Al2O 3And sodium silicoaluminate；
(4) filtrate that step (1) and (2) are collected is mixed, using hydrochloric acid and sulfuric acid tune pH to 7, obtains liquid process hides use
Protein filling, or it is dried to obtain solid-state process hides protein filling.
Embodiment 7
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 6 parts of NaOH, 3 parts of KOH, 3 parts of Ca is added
(OH)2, 10 parts of Al2O3, 2 parts of sodium silicoaluminates, 1000 parts of water react 8h at 90 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 1 part of NaOH, 95 parts of water, in 0.4 MPa of pressure, temperature is added
3h is reacted at 170 DEG C, filter and collects filtrate；
(3) filter residue of step (2) is roasted into 3h at 700 DEG C of temperature, obtained powder is back in step (1) and replaces
Al2O3And sodium silicoaluminate；
(4) filtrate that step (1) and (2) are collected is mixed, using hydrochloric acid and phosphoric acid tune pH to 6, obtains liquid process hides use
Protein filling, or it is dried to obtain solid-state process hides protein filling.
Embodiment 8
(1) hair depilation recycling ox hair is protected in 100 parts of process hides to be placed in reactor, 16 parts of NaOH, 5.5 parts of embodiments 1 is added
The powder that step (3) obtains, 800 parts of water react 10h at 90 DEG C of temperature, filter and collect filtrate；
(2) filter residue of step (1) is placed in reactor, 2 parts of KOH, 100 parts of water, in pressure 0.2MPa, temperature is added
5h is reacted at 130 DEG C, filter and collects filtrate；
(3) filter residue of step (2) is roasted into 2h at 800 DEG C of temperature, obtained powder is back in step (1) and replaces in fact
Apply the powder that 1 step of example (3) obtains；
(4) filtrate that step (1) and (2) are collected is mixed, using hydrochloric acid tune pH to 6, obtains liquid process hides and filled out with albumen
Material, or solid-state process hides protein filling will be obtained after liquid process hides protein filling drying.
Color the same manner as in Example 1 is had also been made to embodiment 2-8 gains (mixed filtrate of step (1) and (2) collection)
Value of chromatism measurement, the result and no significant difference of measurement result and embodiment 1 are spent, therefore no longer does to apply herein and state.
Claims (3)
1. a kind of method for protecting hair depilation recycling ox hair preparation process hides protein filling with process hides, it is characterised in that this method includes
Following processing step:
(1) by weight, 100 parts of guarantor's hair depilation recycling ox hairs are placed in reactor, 6-20 parts of highly basic, 4-10 parts of alkali is added
Property oxide, 0.5-2 parts of sodium silicoaluminates, 500-1000 parts of water react 3-10h at 70-90 DEG C of temperature, filter and collect filter
Liquid；The basic anhydride are MgO, CaO and Al2O3At least one of；
(2) by weight, the filter residue of step (1) is placed in reactor, 0.5-2 parts of highly basic is added, 50-100 parts of water are being pressed
Strong 0.2-0.8MPa reacts 1-5h at 130-190 DEG C of temperature, filters and collect filtrate；
(3) filter residue of step (2) is roasted into 1-4h at 500-800 DEG C of temperature, obtained powder is back in step (1) and replaces
Basic anhydride and sodium silicoaluminate；
(4) filtrate collected in step (1) and (2) is mixed, using inorganic acid tune pH to 5.5-7.5, obtains liquid process hides use
Protein filling, or solid-state process hides protein filling will be obtained after liquid process hides protein filling drying.
2. a kind of method for protecting hair depilation recycling ox hair preparation process hides protein filling with process hides according to claim 1,
It is characterized in that the highly basic is NaOH, Ca (OH)2At least one of with KOH.
3. a kind of method for protecting hair depilation recycling ox hair preparation process hides protein filling with process hides according to claim 1,
It is characterized in that the inorganic acid is at least one of hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid.
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| CN108342524B (en) * | 2018-03-05 | 2020-06-12 | 嘉兴学院 | Resource utilization method of waste animal hair, vinyl retanning material based on keratin hydrolysate and application |
| CN111793726B (en) * | 2020-07-23 | 2022-04-29 | 嘉兴学院 | Method for preparing leather retanning agent by taking waste animal hair as raw material |
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| CN101260141A (en) * | 2008-04-29 | 2008-09-10 | 四川大学 | Method for preparing protein filling material for leather preparation by using leather preparation chromium-containing leftover material as raw material |
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| CN101260140A (en) * | 2008-04-29 | 2008-09-10 | 四川大学 | Method for preparing protein filling material for leather preparation by using animal hair as raw material |
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