CN1760377A - Composition of tanning agent containing modified tara mimosa extract, and bating method without chrome - Google Patents
Composition of tanning agent containing modified tara mimosa extract, and bating method without chrome Download PDFInfo
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- CN1760377A CN1760377A CN 200510021997 CN200510021997A CN1760377A CN 1760377 A CN1760377 A CN 1760377A CN 200510021997 CN200510021997 CN 200510021997 CN 200510021997 A CN200510021997 A CN 200510021997A CN 1760377 A CN1760377 A CN 1760377A
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Abstract
A tanning agent containing modified Tara tannin extract contains proportionally modified Tara tannin extract, non-Cr metal salt and organic phosphorus salt. Its tanning method features that the bare leather must be immersed in acid before tanned.
Description
One, technical field
The present invention relates to a kind of modified tara mimosa extract composition of tanning agent and bating method without chrome thereof, belong to afforestation product in the process hides application in engineering.
Two, background technology
After it is found that chromic salts has good tanning performance, the leather of chromic salts tanning has higher moisture-proof thermostability, good flexibility and fullness, and good water-fast, chemical-resistant reagent and microbial process performance, and occupy dominant position always, up to now, also fail to search out effective substitute products of chrome tanning agent.But chromium causes people's great attention to environment, people and animals' harm problem already, as sexavalent chrome problem in the chromium content in the leather-making waste water, the finished leather.On the one hand traditional chrome tanning method exists the chromium absorption rate low, is generally 60%～80%, has 1/3 chromium to enter in the waste water approximately, causes the pollution to environment and water resources.On the other hand, produce a large amount of chrome leather scraps, these chrome shavinges can't further utilize, and have also increased the weight of environmental pollution.Sexavalent chrome is the international first batch of carinogenicity material of announcing, some developed countries have clearly proposed not contain chromium cpd in some leather goods.Therefore exploitation replaces chrome tanning agent, realizes the pollution-free process for tanning that cleans of no chromic tanning, or effectively solves chrome uptake and combine problem, has become current tanning industry and has pressed for most one of significant problem of solution.
Tannin extract is meant the important afforestation product of a class that obtains with flooding from plant, it is the general name of the mixture of a big class phenolic compound, mainly be present in the cell of tissue such as trunk, bark, leaf, root, shell and fruit of higher plant, plant belongs to renewable resources, particularly tower draws the plant beanpod, can be under the situation of not cutting down plant annual results, and be subjected to people's great attention.
It is a kind of leguminous plants that tower draws, and has another name called Caesalpinia spinosaKuntze (Caesalpinia spinosa), and tower draws the fruit pod to be rich in talas of tannic acid (about 50%～60%).Talas of tannic acid belongs to the tannins tannin in the typical hydrolysable tannins, and it is the quininic acid ester mixture of Nutgalls acyl and poly-Nutgalls acyl, and average empirical formula is C
35H
28O
32, its chemical structure is equivalent to a quininic acid in conjunction with 4～5 galloyls.It is a kind of excellent leather tanning agent, and the finished leather of tanning is than consolidation, and unit elongation is less, and the finished leather color is cream-coloured, and the flat thin property of flexibility, fullness and grain is better.
The prerequisite of any chrome-free tanning is: the performance of (1) finished leather is approaching or reach chrome-tanned standard, and (2) compliance with environmental protection requirements is not introduced new poisonous, objectionable impurities, and (3) its tannery must be economical and practical.
At present, the research of chrome-free tanning agent tannage can be divided into two classes simply, one class is a major objective with the shrinkage temperature of finished leather, this class research is many tans based on the combination of non-chromium metal and organic tanning agent or synthetic polyphenol, combine and tan with Al, Ti, Zn plasma as organic tanning agent, the synergy of these tanning agent tannages can make the shrinkage temperature of finished leather meet or exceed 100 ℃; Another kind of is that the combination of no metal tanning agent and organic tanning agent is tanned or independent organic tanning agent is tanned, combine Rou, oxazolidine with aldehyde as vegetable tanning agent and tan separately, this class tanning agent tannage finished leather shrinkage temperature near or reach 90 ℃.Two class tanning agent tannages respectively have characteristics, and last class replaces chromium can obtain higher shrinkage temperature with non-chromium metal, and shortcoming is that the flexibility and the physical technique performance of finished leather is difficult to stablize, and the usage quantity of neutral salt can not lacked than chrome tanning in the technological process; Back one class finished leather is comparatively soft, and the neutral salt that uses in the process implementing process is less, and shortcoming is that shrinkage temperature is lower.
As far back as the sixties in 20th century, abroad just the someone proposes, can use organophosphorated salt with the organic compound of phenols and various trivalent nitrogens as tanning agent.This was proposed at that time and did not draw attention, and just it simply was classified as the aldehyde tannage class, and did not add to comprehend, and also never tried out.Reason is that when the hazardness that fashion is not realized chromium, people's environmental consciousness is also thinner.Along with people have increasing understanding to this class tanning agent, it just begins as a kind of effective sanitas and linking agent and is studied, and is applied in the curriery.Early 1990s, companies such as Clariant are studied organophosphorated salt once more as a kind of organic tanning agent.Through the application development in more than tens years, proved that the synthetic tanning agent that contains organic microcosmic salt is very promising aspect the production light leather.
With the organophosphorated salt is that tanning agent has the irreplaceable advantage of many other no chromic tannings:
1. organophosphorated salt is a kind of tanning agent of pure natural, and neither containing metal does not contain formaldehyde again, can not bring any pollution in process of production.
2. tanned crust leather is the pure white white wet leather of color, by different retanning dyeing and finishings, can produce high-grade white leather and light color leather, can make brightly painted colored leather again.
3. the leather of tanning has good flame retardant property.
4. containing metal not in the finished leather can be made the metal-free special leather products of ask for something.As glove for golf game leather, high-grade automobile leather etc.Its products waste is biodegradable, can not pollute environment.
The organophosphorated salt tanning agent also has its shortcoming: the price comparison height of one side tanning agent, the unit elongation of finished leather is bigger on the other hand, not too is fit to make sofa artificial leather.And use an amount of tara mimosa extract can overcome the shortcoming of organophosphorated salt tanning.
Three, summary of the invention
The objective of the invention is to provide the method for a kind of modified tara mimosa extract composition of tanning agent and chrome-free tanning thereof at the deficiencies in the prior art, be characterized in tara mimosa extract and non-chromium metal-salt or tara mimosa extract and organophosphorated salt, carry out in conjunction with tanning, by the shrinkage temperature of institute's tanning base being measured and the sense organ of finished leather, the assessment of physical technique performance.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
The recipe ingredient that contains the modified tara mimosa extract composition of tanning agent contains by weight:
100 parts of pickled pelts
5～30 parts of modified tara mimosa extracts
0～13 part of non-chromium metal-salt
0～8 part of organophosphorated salt
Wherein, non-chromium metal-salt and organophosphorated salt can not be zero simultaneously.
The extraction of tara mimosa extract and modification are that the tower with moisture content＜10% draws 100 parts in beanpod powder to add 500 parts in water, 2～8 parts of sodium bisulfites, 0～3 part of S-WAT, 0.5～1.5 part of nonionogenic tenside, in 40～60 ℃ of reactions of temperature 3～5 hours, cavitation process is 20～40 minutes under the ultrasonic wave effect, ultrasonic power 400～1500W, frequency 2 * 10
4～10
9Hz separates vat liquor, through concentrated, dry, obtains the rice white modified tara mimosa extract.
Non-chromium metal-salt is at least a in Tai-Ace S 150, al alum, aluminium chlorohydroxide, titanium tetrachloride, zinc sulfate and/or the rare-earth salts.
Organophosphorated salt is tetra methylol sulfuric acid phosphorus or Tetrakis hydroxymethyl phosphonium chloride.
The process for tanning that contains the modified tara mimosa extract composition of tanning agent, wherein said raw material may further comprise the steps by weight:
1. modified tara mimosa extract combines tanning with non-chromium metal-salt
(1) with 100 parts of pickled pelts, give for 0～13 part with non-chromium metal-salt earlier and tanning, regulate pH=4.0～5.0, after going part to give the waste liquid of tanning, remaining liquor ratio is 40 parts, adds 5～30 parts of modified tara mimosa extracts, changes 1～6 hour, per hour changeed later on 10 minutes, totally 5～10 times, stop drum and spend the night, changeed next day 30～60 minutes, go out drum and leave standstill, record leather base shrinkage temperature and reach more than 90 ℃; Or
(2) with 100 parts of pickled pelts, earlier with 8～25 parts modified tara mimosa extract tanning 6～20 hours, 40～100 parts of liquor ratios, initially pH=4.8～5.6; Add that 0.5～13 part of non-chromium metal-salt is tanned or fixing again, changeed 2～4 hours, go out drum, record the finished leather shrinkage temperature and reach 82～90 ℃, the back of tanning is removed from office base and is carried out rinsing, stuffing according to a conventional method;
2. modified tara mimosa extract combines tanning with organophosphorated salt
(1) modified tara mimosa extract and organophosphorated salt substep tanning
With 100 parts of pickled pelts, 0～8 part of organophosphorated salt, tanning 2～4 hours, body lotion pH=3.5～4.0, with selenium indicator inspection infiltration fully, carry alkali to pH=4.8～6.0 with sodium bicarbonate, drip, washing, with 0.5～3.0 part hydrogen peroxide oxidation 0.5～1.5 hour, add 5～30 parts of modified tara mimosa extracts, tanning 2～6 hours records the finished leather shrinkage temperature and reaches 78～85 ℃; Or
(2) modified tara mimosa extract and organophosphorated salt are with bathing tanning
With 100 parts of pickled pelts, transfer pickling liquid pH to 3.5～4.0,100 parts of liquor ratios, add 0～8 part of organic microcosmic salt, changeed 2～4 hours, the selenium indicator is checked full impregnated, sodium bicarbonate 3～5 ω t% carry pH to 4.5～6.0, add 5～30 parts of modified tara mimosa extracts, change 2～6 hours, check the infiltration situation, add formic acid and regulate pH to 3.8～4.5, stop drum and spend the night, changeed next day 30～60 minutes, washing added 0.5～3 part of hydrogen peroxide oxidation 0.5～2 hour.Record the finished leather shrinkage temperature and reach 78～85 ℃.
The leather color of institute of the present invention tanning is light, soft and full, and grain is flat thin, and Ts reaches 90 ℃.Main physical mechanical skill performance meets China National Light Industrial Products Department's process hides standard promulgated by the ministries or commissions of the Central Government.
The present invention has following characteristics:
1. to draw the beanpod of plant be raw material to the tower of introducing a fine variety with China, the method of sulphite is added in employing in leaching process, realize the technology that efficient lixiviate (ultrasonic cavitation processing) combines with chemical modification synchronously, the preparation modified tara mimosa extract, can increase the raising amount of tannin extract, can improve the solvability and the perviousness of tara mimosa extract again, the aufhellung color.
2. developed the chrome-free tanning technology, particularly combined tanning with aluminium salt or organophosphorated salt, obtained good tanning effect and finished leather performance (comprising organoleptic properties and physicals), reached the physics and chemistry requirement of relevant leather product, Ts reaches 90 ℃.
3. gained finished leather color is light, is beige, and intensity is higher, and fullness is good, and softness is preferably arranged, and can satisfy the requirement of special leather product.
4. avoid the use chromic salts, can not produce the emission problem of chromium in process of production, also do not had chromium or chromic problem in the finished product leather, met the requirement of ecological leather fully.
Four, embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this present embodiment only is used for the present invention is further detailed; but can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can do some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
Pickling ox-hide (cuing open layer thickness 1.8mm), 100kg in pickling liquid, liquor ratio 50kg, add aluminium chlorohydroxide 3kg, changeed 2 hours, and adjusted pH most 5.0～5.2, add tara mimosa extract 10kg with Sulfothiorine or sodium bicarbonate, rotate 6 hours (rotating speed 4rpm), add tara mimosa extract 10kg again, changeed 8 hours, stop drum and spend the night, changeed next day 1 hour, and went out drum and left standstill 2 days.
Rinsing: 150 ω t% water, sulfuric acid 0.8 ω t% (1: 20 times of dilution) changeed 40 minutes (8～10rpm).
Stuffing: add and mix sulfated castor oil 3 ω t% and TRUPON SR 4 ω t%, changeed 90～120 minutes, add the rare-earth salts of 0.5 ω t%, changeed 30 minutes.
Washing: 200% water, changeed 30 minutes.
Drying, the back arrangement.
Become flat thin, the consolidation of grain, fullness is good, and certain flexibility is arranged, and Ts can reach more than 90 ℃.
Embodiment 2
(cut open layer thickness 1.8～2.0mm), 100kg uses the Sulfothiorine disacidify to the pickling pigskin in pickling liquid, transfer pH to 5.2～5.4, add NF synthetic tanning agent 3 ω t%, changeed 1 hour, add tara mimosa extract 10kg, change 6 hours (rotating speed is 4rpm), add tara mimosa extract 14kg again, changeed 6～8 hours, add titanium sulfate tanning agent 1kg, changeed 2 hours, and went out drum and leave standstill, more than 2 days
Stuffing: water 150kg, 35 ℃, CNS synthetic fat liquor 4 ω t%, L-3 fatting agent 3 ω t%.
Fixing: formic acid 1kg, the dilution back is divided three times and is added 60 minutes total times.
Dry, back arrangement.
The finished leather consolidation, plentiful, color is light, and Ts reaches 89 ℃.
Embodiment 3
Goatskin 100kg after softening, without pickling, pH is 6.5～8.0, liquor ratio 100kg adds zinc sulfate 10kg, changes 1～2 hour, adds tara mimosa extract 15kg, changes 5～10 hours, goes out drum and leaves standstill.
Rinsing: adjust about pH to 4.0 with sulfuric acid 1 ω t%.
Stuffing: with CNS synthetic fat liquor 1 ω t%, OS fish-oil stuffing agent agent 3 ω t%, TRUPON EIR 3 ω t% stuffings, arrangement.
Finished leather is soft, plentiful, and shrinkage temperature reaches 80～85 ℃.
Example 4 (after the organophosphorated salt tanning, the tara mimosa extract retanning)
The liming cattle hide cuts open layer (thickness 1.4mm), 100kg (as following materials foundation)
Deliming: water 100kg, 30 ℃, sodium bisulfite 1kg, formic acid 0.3kg changeed 90 minutes, terminal point pH=8.0～8.4 washings
Softening: water 120kg, 37 ℃, trypsinase 0.2kg changeed 90 minutes.
Washing
Pickling: water 100kg, normal temperature, salt 6kg changeed 10 minutes, added formic acid 0.8kg, changeed 30 minutes, added sulfuric acid 0.4kg, changeed 60 minutes, required pH=3.6～3.8.
Organophosphorated salt is tanned: in pickle bath, and tetra methylol sulfuric acid phosphorus 2kg, tanning 4 hours with selenium indicator inspection infiltration fully, is carried alkali to pH=4.8～5.0 with sodium bicarbonate then, drips.
Washing
Oxidation: water 70kg, add hydrogen peroxide 1kg, changeed 40～60 minutes.
Vegetable tanning: add modified tara mimosa extract 10kg, changeed 120 minutes.
Washing
Stuffing: TRUPON EIR 2 ω t%, TRUPON DB 2 ω t%, TRUPON OST 2 ω t%, changeed 60 minutes.Finished leather is consolidation comparatively, and 78～85 ℃ of shrinkage temperatures, tensile strength are 10.2～18.9N/mm
2
Example 5 (organophosphorated salt～tara mimosa extract is with bathing tanning)
Liming goatskin: weigh and make following consumption foundation.
The pelt pre-treatment is with example 1.Transfer pickled pelt pH to 3.7～4.0, liquor ratio 80kg adds organic microcosmic salt 2.5kg, changes 3 hours, and the selenium indicator is checked full impregnated.
The about 3kg of sodium bicarbonate carries pH to 5.0～6.0, adds tara mimosa extract 8kg, changes 5 hours, checks the infiltration situation, adds formic acid 1.2kg, transfers pH to 3.8～4.5, stops drum and spends the night.
Changeed washing, oxidation (with example 1) next day 30～60 minutes.
Tanned leather base is washed, stuffing (with embodiment 4), and drying, the back arrangement gets finished product.The finished leather shrinkage temperature reaches 79～87 ℃ of colors and is beige, and good fullness and elasticity are arranged, better softness, and grain is flat thin.The tensile strength of leather is 11.3～20.1N/mm.
Annotate: sulfated castor oil, CNS synthetic fat liquor, the agent of OS fish-oil stuffing, NF synthetic tanning agent are produced by chemical plant, Wangjiang, Chengdu, and the L-3 fatting agent is produced by chemical plant, booth river, Shifang.Remaining is (Germany) Tang Pule company and produces.
Claims (5)
1. contain the modified tara mimosa extract composition of tanning agent, it is characterized in that the recipe ingredient of said composition tanning agent contains by weight:
100 parts of pickled pelts
5～30 parts of modified tara mimosa extracts
0～13 part of non-chromium metal-salt
0～8 part of organophosphorated salt
Wherein, non-chromium metal-salt and organophosphorated salt can not be zero simultaneously.
2. according to the described modified tara mimosa extract composition of tanning agent that contains of claim 1, it is characterized in that the extraction of tara mimosa extract and modification are that tower with moisture content＜10% draws beanpod powder 100 weight parts to add water 500 weight parts, sodium bisulfite 2-8 weight part, S-WAT 0-3 weight part, nonionogenic tenside 0.5～1.5 weight part, in 40～60 ℃ of reactions 3～5 hours, the cavitation place was 20～40 minutes under the ultrasonic wave effect, ultrasonic power 400～1500WHz, frequency 2 * 10
4～10
9Hz separates vat liquor, through concentrated, dry, obtains the rice white modified tara mimosa extract.
3. according to the described modified tara mimosa extract composition of tanning agent that contains of claim 1, it is characterized in that non-chromium metal-salt is at least a in Tai-Ace S 150, al alum, aluminium chlorohydroxide, titanium tetrachloride, zinc sulfate and/or the rare-earth salts.
4. require the described modified tara mimosa extract composition of tanning agent that contains according to claim 1, it is characterized in that organophosphorated salt is tetra methylol sulfuric acid phosphorus or Tetrakis hydroxymethyl phosphonium chloride.
5. according to the described bating method without chrome that contains the modified tara mimosa extract composition of claim 1, it is characterized in that the described raw material of this method by weight, may further comprise the steps:
1) modified tara mimosa extract combines tanning with non-chromium metal-salt
(1) with 100 parts of pickled pelts, give for 0～13 part with non-chromium metal-salt earlier and tanning, regulate pH=4.0～5.0, after going part to give the waste liquid of tanning, remaining liquor ratio is 40 parts, adds 5～30 parts of modified tara mimosa extracts, changes 1～6 hour, per hour changeed later on 10 minutes, totally 5～10 times, stop drum and spend the night, changeed next day 30～60 minutes, go out drum and leave standstill, record leather base shrinkage temperature and reach more than 90 ℃; Or
(2) with 100 parts of pickled pelts, earlier with 5～30 parts modified tara mimosa extract tanning 6～20 hours, 40～100 parts of liquor ratios, initially pH=4.8～5.6; Add that 0～13 part of non-chromium metal-salt is tanned or fixing again, changeed 2～4 hours, go out drum, record the finished leather shrinkage temperature and reach 82～90 ℃, the back of tanning is removed from office base and is carried out rinsing, stuffing according to a conventional method;
2) modified tara mimosa extract combines tanning with organophosphorated salt
(1) modified tara mimosa extract and organophosphorated salt substep tanning
With 100 parts of pickled pelts, 0～8 part of organophosphorated salt, tanning 2～4 hours, body lotion pH=3.5～4.0, with selenium indicator inspection infiltration fully, carry alkali to pH=4.8～6.0 with sodium bicarbonate, drip, washing, with 0.5～3.0 part hydrogen peroxide oxidation 0.5～1.5 hour, add 5～30 parts of modified tara mimosa extracts, tanning 2～6 hours records the finished leather shrinkage temperature and reaches 78～85 ℃; Or
(2) modified tara mimosa extract and organophosphorated salt are with bathing tanning
With 100 parts of pickled pelts, transfer pickling liquid pH to 3.5～4.0,40～100 parts of liquor ratios, add 0～8 part of organic microcosmic salt, changeed 2～4 hours, the selenium indicator is checked full impregnated, sodium bicarbonate is carried pH to 4.5～6.0 for 3～5 parts, adds 5～30 parts of modified tara mimosa extracts, changes 2～6 hours, check the infiltration situation, add formic acid and regulate pH to 3.8～4.5, stop drum and spend the night, changeed next day 30～60 minutes, washing adds 0.5～3 part of hydrogen peroxide oxidation 0.5～2 hour.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105803134A (en) * | 2014-12-29 | 2016-07-27 | 焦作隆丰皮草企业有限公司 | Sheep leather tanning method |
| CN107447063A (en) * | 2017-08-23 | 2017-12-08 | 成都森钰泓绿化工程有限公司 | A kind of rare earth modified vegetable tanning agent and preparation method thereof |
| CN108165680A (en) * | 2018-03-05 | 2018-06-15 | 焦作隆丰皮草企业有限公司 | A kind of synthesis tanning agent and fur for fur does not dry-clean chrome-free tanning technique |
| CN108193003A (en) * | 2017-12-29 | 2018-06-22 | 齐鲁工业大学 | The preparation method of multi-functional organophosphor tanning agent containing metal |
| CN108624726A (en) * | 2018-04-24 | 2018-10-09 | 安徽乐踏鞋业有限公司 | A kind of preparation method for the vegetable tanning agent that shrinkage temperature is high |
| CN114410856A (en) * | 2022-02-24 | 2022-04-29 | 四川大学 | Chromium-free combined main tanning technology for ecological leather |
| CN114410854A (en) * | 2022-02-24 | 2022-04-29 | 四川大学 | High-temperature-dyeable ecological fur chrome-free combined main tanning process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105803134A (en) * | 2014-12-29 | 2016-07-27 | 焦作隆丰皮草企业有限公司 | Sheep leather tanning method |
| CN105803134B (en) * | 2014-12-29 | 2017-10-10 | 焦作隆丰皮草企业有限公司 | A kind of process for tanning of sheepskin |
| CN107447063A (en) * | 2017-08-23 | 2017-12-08 | 成都森钰泓绿化工程有限公司 | A kind of rare earth modified vegetable tanning agent and preparation method thereof |
| CN108193003A (en) * | 2017-12-29 | 2018-06-22 | 齐鲁工业大学 | The preparation method of multi-functional organophosphor tanning agent containing metal |
| CN108193003B (en) * | 2017-12-29 | 2020-04-28 | 齐鲁工业大学 | Preparation method of multifunctional metal-containing organic phosphorus tanning agent |
| CN108165680A (en) * | 2018-03-05 | 2018-06-15 | 焦作隆丰皮草企业有限公司 | A kind of synthesis tanning agent and fur for fur does not dry-clean chrome-free tanning technique |
| CN108165680B (en) * | 2018-03-05 | 2020-10-09 | 焦作隆丰皮草企业有限公司 | Comprehensive tanning agent for fur and non-dry-cleaning and chrome-free tanning process for fur |
| CN108624726A (en) * | 2018-04-24 | 2018-10-09 | 安徽乐踏鞋业有限公司 | A kind of preparation method for the vegetable tanning agent that shrinkage temperature is high |
| CN114410856A (en) * | 2022-02-24 | 2022-04-29 | 四川大学 | Chromium-free combined main tanning technology for ecological leather |
| CN114410854A (en) * | 2022-02-24 | 2022-04-29 | 四川大学 | High-temperature-dyeable ecological fur chrome-free combined main tanning process |
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| CN100355907C (en) | 2007-12-19 |
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