CN105670815B - A kind of tea seed cleanser and its preparation process - Google Patents

A kind of tea seed cleanser and its preparation process Download PDF

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Publication number
CN105670815B
CN105670815B CN201610020051.XA CN201610020051A CN105670815B CN 105670815 B CN105670815 B CN 105670815B CN 201610020051 A CN201610020051 A CN 201610020051A CN 105670815 B CN105670815 B CN 105670815B
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Prior art keywords
cake
filter residue
camellia oleifera
drying
tea seed
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CN201610020051.XA
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Chinese (zh)
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CN105670815A (en
Inventor
常银子
仲山民
王超
郑剑
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Zhejiang A&F University ZAFU
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Zhejiang A&F University ZAFU
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/662Carbohydrates or derivatives
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/38Products with no well-defined composition, e.g. natural products
    • C11D3/382Vegetable products, e.g. soya meal, wood flour, sawdust
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/50Perfumes

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Detergent Compositions (AREA)
  • Cosmetics (AREA)

Abstract

A kind of tea seed cleanser through drying, crushing, extraction de-oiling, filters using the cake of camellia oleifera seeds after squeezing as raw material, obtains the processes such as re-dry, crushing, packaging after filter residue, finally obtain product.It is up to 98.21% using the technique grease removal efficiency;Saponin content 15.32%, moisture 6.88%, meets product standard;Up to 17.32, brown, uniform free from admixture does not lump, free from extraneous odour, has camellia smell prepared tea seed cleanser detergency.

Description

A kind of tea seed cleanser and its preparation process
Technical field
The invention belongs to plant wastes to utilize technical field, and in particular to a kind of tea seed cleanser and its prepare work Skill.
Background technology
Tea-cake dregs are camellia seed kernels through oil expression a treated blob of slag, about 500,000 tons of the cake of camellia oleifera seeds of the annual output in China, absolutely It is mostly used in feed or is directly dropped.Tea Saponin containing 10%-13% in cake of camellia oleifera seeds is a kind of natural table of function admirable Face activating agent has the properties such as good emulsification, dispersion, moistening, foaming, foam stabilizing, decontamination, but at present not yet by reasonable development.
Invention content
For the above problem present in background technology, the object of the present invention is to provide a kind of tea seed cleanser and its systems Standby technique, i.e., prepare a kind of tea seed powder that dirt-removing power is strong by raw material of cake of camellia oleifera seeds.
The technical solution adopted by the present invention is as follows:
A kind of tea seed cleanser, it is characterised in that it is prepared by following technique:
1)Raw material selects:Select the cake of camellia oleifera seeds after squeezing for raw material;
2)Pretreatment of raw material:The impurity in cake of camellia oleifera seeds is removed, drying to constant weight through 50 DEG C, smashes it through 40 mesh sieve, 50- 60 DEG C of dryings to moisture is less than 3%, obtains cake of camellia oleifera seeds powder;
3)Extract de-oiling:Cake of camellia oleifera seeds powder is weighed, is placed in Soxhlet extractor, using petroleum ether as solvent, in extraction temperature Spend 50 DEG C, solid-liquid ratio 1:5(M:V)Under the conditions of extract 3h;Then it is filtered at vacuum degree 0.06-0.08MPa, retains filter residue;
4)Filter residue and drying:Filter residue is placed in baking oven dry 2-4 h under the conditions of 70-90 DEG C;Preferably:70 DEG C of dry 3h;
5)Filter residue crushes:Filter residue after drying is smashed it through into 60 mesh sieve again, obtains tea seed cleanser;
6)Packaging:Obtain finished product.
A kind of application of the above-mentioned tea seed cleanser on cleaning clothing.
Using above technical scheme, grease removal efficiency is up to 98.21%, saponin content 15.32%, obtained tea seed is gone For the detergency of dirty powder up to 17.32, dirt-removing power has pole to dramatically increase than founding white liquid detergent(p<0.01);The acid-base value of tea seed powder Be more suitable for the skin of human body, the irritation of opponent is small, modest viscosity, product is brown, uniform free from admixture, do not lump, free from extraneous odour, With camellia smell.
Description of the drawings
Fig. 1:Influence of the extraction temperature to grease removal efficiency in cake of camellia oleifera seeds;
Fig. 2:Influence of the extraction time to grease removal efficiency in cake of camellia oleifera seeds;
Fig. 3:Influence of the solid-liquid ratio to grease removal efficiency in cake of camellia oleifera seeds;
Fig. 4:Influence of the granular size to detergency in cake of camellia oleifera seeds.
Specific implementation mode
Below by specific embodiment, the present invention is described in further detail.
Embodiment 1
(1)MATERIALS METHODS
Raw material and reagent
Cake of camellia oleifera seeds:Resid amount 9.14%, Jinhua, Zhejiang Kingsoft grease Co., Ltd.
Reagent:Tea Saponin standard items:Purity 98%, Shanghai Yuan Ye Bioisystech Co., Ltd;Petroleum ether(Boiling range 30-60 ℃), vanillic aldehyde, absolute ethyl alcohol, sulfuric acid etc. is that analysis is pure.
Equipment
HR 1727/06/BC type blenders, HH-4 type digital display thermostat water baths, DK-S26 type electric-heated thermostatic water baths, DGG-9053AD type electric heating constant-temperature blowing drying boxes, 7220 type spectrophotometers of VIS-, 40 mesh, 60 mesh, 80 mesh, 100 mesh, 120 Mesh standard sieve, ZK-801 type mini desktop vacuum pumps, RE-2000 Rotary Evaporators, NDJ-5s type rotational viscometers.
Test method
Index and performance measurement
Fat:With reference to GB/T5009.6-2003《Fatty measurement in food》;Saponin:According to vanillic aldehyde-sulphate method inspection Survey the content of Tea Saponin;Moisture:With reference to GB 50093-2010《The measurement of moisture in food》It carries out;Detergency:With reference to Zhang Shixin Detergency experiment carries out;PH value measures:Clean product solution is washed in preparation 1%, is measured using pH meter;Stability Determination:Stability (Fluid product)It is placed in -3-10 DEG C of refrigerator for 24 hours, takes out the when of restoring to room temperature and observe nodeless mesh, no precipitation;(40±1) DEG C incubator in place for 24 hours, taking-up observe immediately it is not stratified, it is haze-free, and do not change smell;Viscosimetric analysis:It takes suitable Test specimen pours into 200 milliliters of beaker in tall form, with turning viscosimeter determination sample in 0 DEG C, 25 DEG C, 40 DEG C of viscosity.
Technological process
Cake of camellia oleifera seeds → drying → crushing → extraction de-oiling → suction filtration(It is concentrated in vacuo, vacuum degree 0.06-0.08MPa)→ filter Slag → filter residue and drying → filter residue crushing → packaging → product
Pretreatment of raw material:The impurity in cake of camellia oleifera seeds is removed, drying to constant weight through 50 DEG C, smashes it through 40 mesh sieve, 50-60 DEG C drying(Final moisture content<3%).
Extract de-oiling:A certain amount of cake of camellia oleifera seeds powder is weighed, is placed in Soxhlet extractor, using petroleum ether as solvent, is ground Study carefully the influence that extracting condition washes cake of camellia oleifera seeds grease removal efficiency in clean product.
Process optimization
1.3.3.1 grouts Residual oil technique
In de-oiling technique, using grease removal efficiency as index, extraction temperature is studied(30-60℃), extraction time(2-8h)、 Solid-liquid ratio(m:V, 1:3-1:7)To grease removal efficiency in grouts(Calculation formula is carried out by formula 1)Influence, and it is true with Orthogonal Method Surely the extracting technology of Residual oil in grouts is removed.
Filter residue and drying technique
Using baking oven, drying temperature is studied(50-110℃), drying time(1h-4h)To Tea Saponin content and moisture Influence.
Filter residue crushes
With product particle degree size(40 mesh, 60 mesh, 80 mesh, 100 mesh, 120 mesh)For its shadow to detergency of Elements research It rings.
Data analysis
All experiments 3 times are parallel, are averaged and standard deviation, SPSS17.0 softwares carry out variance analysis.
(2)As a result with analysis
Influence of the extraction temperature to grease removal efficiency in cake of camellia oleifera seeds
The dry oil-tea-cake meal 10g to constant weight is weighed, by solid-liquid ratio 1:5(M:V)It is molten as extracting that petroleum ether is added Agent, respectively under conditions of extraction temperature is 30,40,50,60 DEG C, it is de- to grease to investigate different extraction temperatures by extraction time 3h Except the influence of rate, the result is shown in Figure 1.
As seen from Figure 1, within the scope of 40-50 DEG C, grease removal efficiency increases very fast(p<0.01), and in extraction temperature When degree is 50 DEG C, grease removal efficiency reaches maximum value 98.22%;Continue to increase temperature, grease removal efficiency has small size reduction(p> 0.05).Therefore, 50 DEG C or so of Extracting temperature selection is more suitable.
Influence of the extraction time to grease removal efficiency in cake of camellia oleifera seeds
The dry oil-tea-cake meal 10g to constant weight is weighed, by solid-liquid ratio 1:5(M:V)It is molten as extracting that petroleum ether is added Agent, under conditions of extraction temperature is 50 DEG C, extraction time is respectively 2,3,4,5,6,7,8h, investigate different extraction times
Influence to grease removal efficiency, is as a result shown in Fig. 2.
Extraction time has more significant influence to cake of camellia oleifera seeds grease removal efficiency, and with the extension of extraction time, grease is de- Except rate is continuously improved(p<0.01), for extraction time in 3h, grease removal efficiency reaches 98.26%;Extraction time is more than 3h, grease Removal efficiency amplitude of variation slows down(p>0.05), big many greases of sauce has all been extracted.Therefore, it is more suitable to be selected as 3h for extraction time Preferably.
Influence of the solid-liquid ratio to grease removal efficiency in cake of camellia oleifera seeds
With 50 DEG C of extraction temperature, under conditions of extraction time 3h, research solid-liquid ratio is 1:3、1:4、1:5、1:6、1:7 pairs of oil The influence of tea-cake dregs grease removal efficiency, test result are shown in Fig. 3.
With the increase of petroleum ether dosage, cake of camellia oleifera seeds residua content is reduced, and grease removal efficiency pole dramatically increases(p< 0.01), when solid-liquid ratio is more than 1:When 5, grease removal efficiency tends towards stability(p>0.05), it is 98.23 when grease removal efficiency maximum.
The optimization of cake of camellia oleifera seeds extracting technology
It uses petroleum ether as Extraction solvent, chooses solid-liquid ratio, extraction temperature, three factor of extraction time as influence Oil-tea-cake The principal element of dregs of rice grease removal efficiency, and three factor L are designed with this9(33)Orthogonal test, orthogonal experiment data and analysis result are shown in Table 1.
As shown in Table 1, the principal element sequence for influencing cake of camellia oleifera seeds extracting technology is B > A > C, optimum extraction process Item is A2B2C2, i.e. 50 DEG C of Extracting temperature, solid-liquid ratio 1:5(M:V), extraction time 3h.This optimum process condition combines not Occur in table, so 3 confirmatory experiments are carried out to it, cake of camellia oleifera seeds Residual oil fat removal efficiency average out to 98.21%, higher than above-mentioned Test result shows A2B2C2For optimum extraction condition, grouts residual oil content is 1.89% with this condition<2.0%, meet initially One of product standard of formulation.
Influence of the drying condition to the content of Tea Saponin
Grouts utilizes oven drying, research drying temperature after de-oiling is filtered(50-110℃), drying time(1h-4h) Influence to the content of Tea Saponin and moisture, experimental result are shown in Table 2.
As can be seen from Table 2 under the conditions of different disposal, saponin content and moisture have different degrees of variation.9 Saponin content under a treatment conditions is all higher than 10% and complies with standard, wherein 70 DEG C of dry 3h and 4h highests, but dry 4h compares drying The saponin content variation of 3h is little(p>0.05), while moisture with this condition<8%, meet the technical indicator of product, but In view of economic benefit, therefore final drying condition selects 70 DEG C of drying temperature, time 3h.
Influence of the milling product granularity size to detergency
Grouts after de-oiling are crushed, 40 mesh, 60 mesh, 80 mesh, 100 mesh and 120 mesh sieve, granular size is crossed respectively and corresponds to respectively 0.420mm, 0.250mm, 0.178mm, 0.150mm and 0.124mm, study the influence to product detergency, and measurement result is shown in figure 4。
As seen from Figure 4, as tea seed grouts particle is smaller, detergency improves rapidly(p<0.01), reach 17.32, after being sieved to 60 mesh(Granularity<0.250mm)Tea seed powder detergency effect it is preferable, but amplitude of variation is little(p> 0.05).
Tea seed powder properties of product
The tea seed powder prepared according to optimum process is measured its performance, and measurement result is shown in Table 3.
As can be seen from Table 3, the 1% of same 1kg washes clean solution, and the dirt-removing power of tea seed powder has extremely significantly than founding white liquid detergent Increase(p<0.01);The acid-base value of tea seed powder is more suitable for the skin of human body, and the irritation of opponent is small;Tea seed powder under different temperatures Viscosity differences are very big, and temperature is higher, and viscosity is lower, but after 25 DEG C, and the amplitude that viscosity reduces becomes smaller.Tea seed powder ratio of viscosities is vertical White liquid detergent is low, and the stability of viscosity is relatively poor, but this has no effect on its dirt-removing power, and at normal temperatures, tea seed powder is washed clean The viscosity of product is more moderate.Product is brown, uniform free from admixture, do not lump, free from extraneous odour, has camellia smell.
(3)Conclusion
Using petroleum ether as extraction solvent, it is to carry to remove oil tea to squeeze the optimum process condition of grouts Residual oil by extraction Take temperature 50 C, solid-liquid ratio 1:5(m:V), extraction time 3h, with this condition oil tea squeezing grouts grease removal efficiency be 98.22%, the residual oil content in grouts is only 1.77%(<2.0%).
Under the conditions of 70 DEG C of drying temperature, time 3h, saponin content is 15.32%(>10%), moisture 6.88%(< 8%).
Cross 60 mesh sieve(Granularity 0.250mm)Tea seed powder detergency effect it is preferable, viscosity, stability are than vertical White product is good and smaller to human skin irritation.Final brown, the uniform free from admixture of product does not lump, free from extraneous odour, has Camellia smell.

Claims (4)

1. a kind of tea seed cleanser, it is characterised in that it is prepared by following technique:
1)Raw material selects:Select the cake of camellia oleifera seeds after squeezing for raw material;
2)Pretreatment of raw material:The impurity in cake of camellia oleifera seeds is removed, drying to constant weight through 50 DEG C, smashes it through 40 mesh and sieves, 50-60 DEG C It is dry to be less than 3% to moisture, obtain cake of camellia oleifera seeds powder;
3)Extract de-oiling:Cake of camellia oleifera seeds powder is weighed, is placed in Soxhlet extractor, using petroleum ether as solvent, in Extracting temperature 50 DEG C, solid-liquid ratio 1:5(M:V)Under the conditions of extract 3h;Then it is filtered at vacuum degree 0.06-0.08MPa, retains filter residue;
4)Filter residue and drying:Filter residue is placed in baking oven dry 2-4 h under the conditions of 70-90 DEG C;
5)Filter residue crushes:Filter residue after drying is smashed it through into 60 mesh sieve again, obtains tea seed cleanser;
6)Packaging:Obtain finished product.
2. a kind of tea seed cleanser according to claim 1, it is characterised in that step 4)Middle filter residue and drying condition is:70 DEG C dry 3h.
3. a kind of preparation process of tea seed cleanser, it is characterised in that it mainly includes the following steps:
1)Raw material selects:Select the cake of camellia oleifera seeds after squeezing for raw material;
2)Pretreatment of raw material:The impurity in cake of camellia oleifera seeds is removed, drying to constant weight through 50 DEG C, smashes it through 40 mesh and sieves, 50-60 DEG C It is dry to be less than 3% to moisture, obtain cake of camellia oleifera seeds powder;
3)Extract de-oiling:Cake of camellia oleifera seeds powder is weighed, is placed in Soxhlet extractor, using petroleum ether as solvent, in Extracting temperature 50 DEG C, solid-liquid ratio 1:5(M:V)Under the conditions of extract 3h;Then it is filtered at vacuum degree 0.06-0.08MPa, retains filter residue;
4)Filter residue and drying:Filter residue is placed in baking oven dry 3h under the conditions of 70 DEG C;
5)Filter residue crushes:Filter residue after drying is smashed it through into 60 mesh sieve again, obtains tea seed cleanser;
6)Packaging:Obtain finished product.
4. a kind of application of the tea seed cleanser according to claim 1 or 2 on cleaning clothing.
CN201610020051.XA 2016-01-13 2016-01-13 A kind of tea seed cleanser and its preparation process Expired - Fee Related CN105670815B (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106190609A (en) * 2016-07-05 2016-12-07 武汉轻工大学 The preparation method of high active ingredient tea cake powder detergent and tea cake powder detergent
CN107043658A (en) * 2017-05-15 2017-08-15 湖南农业大学 A kind of evaluation method of duck's egg cleaning agent decontamination bacteria-eliminating efficacy
CN110003999B (en) * 2019-03-25 2021-11-05 苏州优养健康科技有限公司 Camellia seed cleaning powder and preparation process thereof
CN111304662A (en) * 2020-04-10 2020-06-19 湖南淳湘农林科技有限公司 Preparation method of tea seed cake cleaning agent
CN112076878A (en) * 2020-09-01 2020-12-15 湖南杨家将茶油股份有限公司 Method for making tea seed cake food washing product

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1063306A (en) * 1991-10-31 1992-08-05 中国科学院广州化学研究所 Withering tea powder detergent
US7977290B1 (en) * 2008-06-05 2011-07-12 Jeffrey Alan Deane Body cleansing composition
CN102260316A (en) * 2011-05-23 2011-11-30 井冈山茶油有限公司 Method for purifying tea saponin from oil tea seed cake pulp
CN103232902A (en) * 2013-04-25 2013-08-07 覃永良 Camellia saponin detergent powder for removing greasy dirt of natural plants

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1063306A (en) * 1991-10-31 1992-08-05 中国科学院广州化学研究所 Withering tea powder detergent
US7977290B1 (en) * 2008-06-05 2011-07-12 Jeffrey Alan Deane Body cleansing composition
CN102260316A (en) * 2011-05-23 2011-11-30 井冈山茶油有限公司 Method for purifying tea saponin from oil tea seed cake pulp
CN103232902A (en) * 2013-04-25 2013-08-07 覃永良 Camellia saponin detergent powder for removing greasy dirt of natural plants

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