CN105315681A - Preparing method for cottonseed protein biodegradable plastics - Google Patents
Preparing method for cottonseed protein biodegradable plastics Download PDFInfo
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Abstract
The invention relates to a preparing method for biodegradable plastics, in particular to a preparing method for cottonseed protein biodegradable plastics. The preparing method for the cottonseed protein biodegradable plastics includes the steps of extracting cottonseed protein; preparing a cottonseed protein/glycerinum mixture; preparing a cottonseed protein/glycerinum/glutaraldehyde mixture, wherein after the cottonseed protein/glycerinum mixture is prepared, glutaraldehyde is added to react with the cottonseed protein/glycerinum mixture in a hot bath; preparing a cottonseed protein/glycerinum/glutaraldehyde/Na-montmorillonite mixture, wherein a montmorillonite solution purified through a static settlement method is added and fully mixed, and then montmorillonite is added. The cottonseed protein is used as a raw material for preparing the complete biodegradable plastics, and the purpose is to overcome the serious defects that processability, mechanical performance and water resistance of the biodegradable plastics are poor. Starting from physical modification, the processability of the cottonseed protein is improved through glycerinum, in the perspective of chemical modification, the cottonseed protein is subjected to crosslinking modification through glutaraldehyde, and finally montmorillonite is used for filling to improve the mechanical performance and water resistance of the cottonseed protein plastics.
Description
Technical field
The present invention relates to a kind of preparation method of degradative plastics, particularly relate to a kind of preparation method of cottonseed protein degradative plastics.
Background technology
Along with the increase of plastics output, the reduction of cost, people are this type of the plastics such as no longer Reusability commodity bundle pack, fluid container and agricultural mulching just, make this kind of plastics become the class waste product be namely dropped." white pollution " that waste plastic brings, having become one can not unheeded social effects of pollution again
[1].Along with the enhancing of people's environmental protection consciousness, nondegradable petroleum-based plastics will be replaced gradually.In addition, oil is a kind of non-renewable resource, and in the near future, this limited resources can be exploited totally.Therefore, a kind of reproducible resource must be found to replace oil as the raw material producing plastics.
In recent years, protein receives publicity gradually as a kind of non-petroleum, environmental safety, resource that is biodegradable and that can regenerate.In natural polymer, perhaps protein be utilize minimum natural resource in industrial application, and they are considered to be the function in feed and nutritive ingredient substantially, and are familiar with far away as the great potential that structural motif is applied at non-food industries and understand.Cottonseed protein is hydrophilic material inherently, has extremely strong avidity with water molecules, can by hydrogen bond by around the Water Molecular Adsorption of polarity to protein molecular.By carrying out blended, grafting, copolymerization, the modification such as crosslinked to plant animal protein, corresponding protein based materials can be obtained.China is the first in the world Chan Mian big country, and output of cotton accounts for 1/3 of World cotton production, and produce cottonseed about 8,000,000 t per year, carrying the cottonseed meal matter content after oil can reach 38% ~ 45%.Calculate with this, the cotton dregs annual production after oil is proposed more than 4,000,000 t by annual China, about containing protein 1,600,000 t, is a kind of huge plant protein resource.So utilize cottonseed protein to study biodegradable plastic, both took full advantage of the cottonseed meal resource of China's abundant, solved again the white pollution problems that common plastics causes environment.Macromolecular material is applied to every field, is dispersed throughout in our work, study, life ubiquitously, applied range convenient, fast with it and famous.But common high molecular materials is difficult to degraded under field conditions (factors), brings serious pollution to environment.Since entering 21 century, environment of preserving our planet, construct resource recycling society, walk sustainable development path, become World Focusing focus and urgent task.Biodegradable plastic, by the whole life cycle analysis of product, has confirmed as low environmental load material.In addition, the main raw material of quite a few biodegradable plastic is the agricultural resource from can regenerate every year, as limited, day by day reduce, supplementing of increasingly exhausted non-renewable petroleum resources substitute, and also become the development trend of attracting attention in the whole world.Therefore, biodegradable plastic has become the whole world research and development focus, particularly complete biodegradable by current for the emphasis being future development, has a lot of people being all engaged in the research of degradable plastics.
Cottonseed meal is the byproduct of cottonseed after process of deoiling, very low to its utilization ratio in China, is mainly used for pasture.Due to the Cotton Production state that China is maximum, therefore output is very large.With this secondary raw material for raw material, cost is low, is conducive to the acquisition of suitability for industrialized production Raw.And, containing multiple group in cottonseed protein molecule, be conducive to its modification.Therefore, due to oil crisis and a series of environmental problem, its purposes in degradable material field has caused the common concern of people, and this also imply that the broad prospect of application of protein-based biodegradable plastic.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of cottonseed protein degradative plastics, the present invention is that complete biodegradable plastics prepared by raw material with cottonseed protein, be intended to overcome its processing characteristics and mechanical property is not good, the major defects such as poor water resistance, from physically modified, the processibility of cottonseed protein is improved with glycerine, the angle of chemically modification again, carry out cross-linking modified by glutaraldehyde to cottonseed protein, last using polynite as filling, to improving mechanical property and the water tolerance of plastics with cotton seed protein.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for cottonseed protein degradative plastics, described method comprises following process:
First, the extraction of cottonseed protein, select the grouts after cottonseed oil expression of peeling off, pulverize with pulverizer, sieve, getting powder is raw material, treats that next step uses after drying; Take cottonseed meal, measure distilled water, add sodium hydroxide, in a water bath heated and stirred; Extract complete, centrifugation, get supernatant liquid and treat that next step uses; Supernatant liquor hydrochloric acid soln carries out titration, is titrated to the pH value needed for test, stops acid adding, carries out centrifugation, get precipitation, with deionized water wash, be put in air dry oven and carry out drying, obtain cottonseed protein isolate; Then finished product is prepared step by step as follows:
(1) cottonseed protein/glycerine is prepared
By in cottonseed protein, add glycerine, dispersed with stirring; This mixture is imported culture dish, dries in vacuum drying oven;
Sample after drying is molded into sheet on vulcanizing press, then moves in another normal temperature press and cool; Leave standstill in atmosphere after print is cut into test bars, test its properties;
(2) cottonseed protein/glycerine/glutaraldehyde is prepared
After preparing cottonseed protein/glycerol mixture with (1), then add glutaraldehyde, react in hot water bath, add glutaraldehyde; Subsequent process is with method for making sample is consistent above;
(3) cottonseed protein/glycerine/glutaraldehyde/sodium-based montmorillonite is prepared
In (2), add the polynite solution of purifying through quiet settling process in preparation, fully mix, add polynite, subsequent process is with method for making sample is consistent above.
The preparation method of described a kind of cottonseed protein degradative plastics, described glycerine number selects 20 parts/100 parts cottonseed proteins to be good.
The preparation method of described a kind of cottonseed protein degradative plastics, described glutaraldehyde content is 30% of cottonseed protein quality, and when molding temperature is 140 DEG C, the tensile strength of cottonseed protein plastics reaches 17.22MPa, and water-intake rate is also down to 44.8%; The optimum proportioning of glutaraldehyde modification cottonseed protein plastics is cottonseed protein 100 parts, glutaraldehyde 30 parts.
The preparation method of described a kind of cottonseed protein degradative plastics, when described polynite content is 6%, tensile strength is the highest, and be 19.1MPa, water-intake rate is minimum, is 27.8%; Comprehensive Correlation, polynite number should select 6 parts/100 parts cottonseed protein the bests.This
Advantage and the effect of invention are:
The present invention, by using nontoxic, low toxicity and processing modified adjuvant with low cost is processing modified to cottonseed protein, prepares and has higher mechanics mechanical property and water tolerance and cottonseed protein degradative plastics material nontoxic, with low cost.
Accompanying drawing explanation
Fig. 1 is the SEM figure of glycerine plasticising plastics with cotton seed protein;
The XRD figure of Fig. 2 glycerine plasticising plastics with cotton seed protein;
Fig. 3 glutaraldehyde modification cottonseed protein plastics SEM photo;
Fig. 4 a-glycerine plasticising and b-polynite strengthen the infrared spectrogram of glutaraldehyde modification cottonseed protein plastics;
Fig. 5 polynite strengthens the SEM photo of glutaraldehyde modification cottonseed protein plastics.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The extraction of cottonseed protein, select the grouts after cottonseed oil expression of peeling off, pulverize with pulverizer, sieve, getting 200 object powders is raw material, treats that next step uses after dry (40 DEG C, 12h).Take a certain amount of cottonseed meal, measured amounts distilled water (liquid pool is than 12:1), adds the sodium hydroxide (being adjusted to PH=11) of 1mol/L, in a water bath heated and stirred (70 DEG C, 1h).Extract complete, centrifugation (4000r/min, 10min), get supernatant liquid and treat that next step uses.The hydrochloric acid soln of supernatant liquor 1mol/L carries out titration, is titrated to the pH value (PH=4.8) needed for test, stops acid adding.Carry out centrifugation (4000r/min, 10min), get precipitation, with deionized water wash 3 times, be put in air dry oven and carry out drying (50 DEG C, 24h), obtain cottonseed protein isolate.
(1) cottonseed protein/glycerine sample is prepared
By in cottonseed protein, add glycerine (mass ratio of glycerine and protein is respectively 10:1,10:2,10:3,10:4), dispersed with stirring 20min; This mixture is imported culture dish, and in vacuum drying oven, (35 DEG C) dry.
By in blocks for sample (pressure 10MPa, first cold pressing 5min, then constant temperature pressurize 20min, and hot pressing temperature the is 120 DEG C) mold pressing on vulcanizing press after drying, then move in another normal temperature press and cool.Leave standstill 24h in atmosphere after print is cut into test bars, test its properties.
(2) cottonseed protein/glycerine/glutaraldehyde sample is prepared
After preparing cottonseed protein/glycerine (mass ratio is 10:2) mixture with (1), add glutaraldehyde again, reaction 20min in the hot water bath (70 DEG C), the massfraction adding glutaraldehyde be respectively 10%, 20%, 30%, the massfraction of 40%(glutaraldehyde, w/w).Wherein, molding temperature is respectively 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C, 150 DEG C, and subsequent process is with method for making sample is consistent above
(3) cottonseed protein/glycerine/glutaraldehyde/sodium-based montmorillonite sample is prepared
Add the polynite solution of purifying through quiet settling process in G30 of preparation in (2), fully mix 20min, the massfraction adding polynite is respectively 2%, 4%, 6%, 8%, the massfraction of 10%(polynite).Wherein, molding temperature is 140 DEG C, and subsequent process is with method for making sample is consistent above.
Examination of infrared spectrum
Grind compressing tablet with KBr after being pulverized by print, then on FT-IR470 type infrared spectrometer, carry out infrared analysis.
X-ray diffraction adopts D8ADVANCE type x-ray diffractometer, carries out X-ray diffraction analysis respectively by powder diffraction method to each sample after analyzing and being pulverized by print.
Scanning electron microscope test
By the sample section metal spraying after stretching, adopt JSM-6360LV type scanning electron microscopic observation cross-section morphology, and take pictures.
Elongation test
Obtained dumbbell shape batten is directly carried out stretching mechanical property testing on RGL-30A shaped material trier, and draw speed is 10mm/min, and tensile strength unit is MPa.
Water-intake rate is tested
Accurately take a certain amount of sample and put into beaker, add deionized water, soak 24h, then dry the water of sample surfaces with worry paper, weigh.The water-intake rate of sample is calculated by formula (1)
W=(M2—M1)/M1×100%（1）
Wherein: W is the water-intake rate (g/g) of sample; M1 is original quality (g); M2 is the quality (g) after water suction.
Biodegradability is tested
The biological degradability of test piece is tested by soil burial test, is embedded in the dark soil of 20cm after print being contained in nylon porous web, takes out batten in 50 DEG C of dryings until constant weight, then weigh every five days.Circulation like this four times.The rate of weight loss (Wloss) of sample before and after soil buries calculates by formula (2):
Wloss=(M1-M2）/M1×100%（2）
In formula M1 and M2 be respectively sample place into the soil before and after dry weight solubility property test
At room temperature, test piece is soaked in completely and is equipped with in the beaker of distilled water, change water every day once, so circulation one week.Initial print is taken pictures together with print after dissolving and contrasts.
Thermal Synthetic Analysis
The sample powder of 8 ~ 10mg loaded in A12O3 crucible, take N2 as atmosphere, flow is 10ml/min, and temperature rise rate is 10K/min, Range of measuring temp 30 DEG C ~ 810 DEG C.
Dsc analysis
The sample powder of 8 ~ 10mg is loaded in the crucible of aluminum.Take N2 as atmosphere, flow 50ml/min, temperature rise rate 10 DEG C/min, with the empty crucible of aluminum for reference, test specification 40 DEG C ~ 200 DEG C.
The influence factor of cottonseed protein extraction yield
The factor affecting extraction yield mainly contain the pH value of extraction liquid, temperature, the time and liquid pool ratio, but due to liquid pool ratio influence factor little, so mainly have studied these 3 factors to the impact of extraction rate of protein.Wherein, cottonseed meal powder is 30g, and liquid pool is than being 1:12.
Table 1 temperature is on the impact of extraction yield
| T/ DEG C of numbering | 1 | 2 | 3 | 4 | Mean value |
| 40 | 4.912 | 4.463 | 4.619 | 4.846 | 4.710 |
| 50 | 6.095 | 6.253 | 6.638 | 6.578 | 6.391 |
| 60 | 6.340 | 6.257 | 6.543 | 6.321 | 6.365 |
As shown in Table 1, the extraction yield of cottonseed protein raises with the rising of temperature, but when temperature is raised to 60 DEG C, extraction yield change is little.Because temperature crosses high protein meeting sex change, so extraction temperature should select 50 DEG C of the bests.
Table 2 time is on the impact of extraction yield
| T/min numbers | 1 | 2 | 3 | 4 | Mean value |
| 30 | 6.095 | 6.253 | 6.638 | 6.578 | 6.391 |
| 50 | 8.068 | 8.228 | 8.086 | 8.330 | 8.178 |
| 70 | 8.799 | 8.679 | 8.255 | 8.401 | 8.534 |
As shown in Table 2, the extraction yield of cottonseed protein increase in time and raising, but tend towards stability to extraction yield during 70min, and protein decomposed under long-time basic conditions, in process is sunk in acid, be difficult to precipitation completely, cause isoelectric points of proteins place solubleness to increase, extraction yield reduces.So extraction time should select 70min best.
Table 3 Acidity is on the impact of extraction yield
| PH numbers | 1 | 2 | 3 | 4 | Mean value |
| 4.5 | 8.090 | 7.831 | 7.226 | 7.437 | 7.646 |
| 4.8 | 8.799 | 8.228 | 8.086 | 8.330 | 8.178 |
| 5.1 | 7.720 | 7.681 | 7.694 | 7.998 | 7.773 |
As shown in Table 3, concentration of hydrochloric acid is less on extraction rate of protein impact, and as PH=4.8, extraction yield is the highest.
The strong and weak impact on extraction yield of table 4 alkalescence
| PH numbers | 1 | 2 | 3 | 4 | Mean value |
| 10 | 5.123 | 5.971 | 5.368 | 6.011 | 5.618 |
| 11 | 8.632 | 8.377 | 8.901 | 8.472 | 8.600 |
| 12 | 8.661 | 8.253 | 8.139 | 8.862 | 8.479 |
As shown in Table 4, naoh concentration has a significant impact extraction rate of protein, along with naoh concentration increases, extraction rate of protein obviously increases, and when solution pH value reaches 11, extraction yield tends towards stability, in order to prevent protein denaturation, keep again higher extraction yield, pH value selects 11 the bests.
In sum, from table 1, table 2, table 3, table 4, extracting cottonseed protein optimised process is: temperature 50 C, extraction time 70min, pH value is 4.8/11.
The Tensile fracture stereoscan photograph of glycerine plasticising plastics with cotton seed protein is shown in Fig. 1.The fractography layering of batten as can be seen from Figure, and there is the micropore much differed in size, illustrate that the mechanical property of glycerine plasticising plastics with cotton seed protein is very poor, very easily rupture.And because a large amount of micropores exists, so water absorbing properties is very large, easily make moist.This just causes the range of application of material greatly limited, not easily uses.
Fig. 2 is the XRD figure of glycerine plasticising plastics with cotton seed protein.In figure there is obvious sharp diffraction peak near 8 ° and 19 ° in 2 θ, this characteristic peak corresponding after being the crystallization formed after the alpha-helix of cottonseed protein and beta sheet.Illustrate that cottonseed protein is a kind of amorphous state material of crystallization.
The amido linkage peak of glutaraldehyde modification cottonseed protein plastics moves (shifting to 3340cm-1 from 3300cm-1) to high wave number, is because glutaraldehyde and protein generation crosslinking reaction, decreases hydrogen bond action.Further, after glutaraldehyde cross-linking, 1040cm-1 peak is sharpened, and peak moves (shifting to 1040cm-1 from 1070cm-1) to lower wave number, is because the α-helixstructure in protein is opened.Can prove that glutaraldehyde and protein there occurs crosslinking reaction thus.Fig. 3 is the Tensile fracture stereoscan photograph of glutaraldehyde modification cottonseed protein plastics.SEM figure shows the section opposed flattened of cottonseed protein plastics, does not have layering and micropore, and presents structure more in good order, confirms glutaraldehyde and cottonseed protein crosslinking reaction well, can effectively improve its mechanical property, reduce its water-absorbent.
XRD analysis
Fig. 4 is the infrared spectrogram that the plasticising of a-glycerine and b-polynite strengthen glutaraldehyde modification cottonseed protein plastics.Because polynite specific surface area is larger, and can with protein molecule generation electron transfer reaction, so the polar group of polynite very easily adsorbed proteins, so hydrogen bond action can weaken further, therefore, the amido linkage peak value that polynite strengthens glutaraldehyde modification cottonseed protein increases to 3400cm-1 by 3300cm-1, and I band charateristic avsorption band of protein amido linkage increases to 1660cm-1 by 1650cm-1.
Fig. 5 is the Tensile fracture stereoscan photograph that polynite strengthens glutaraldehyde modification cottonseed protein plastics.Show batten section relative smooth in figure, without layering and micropore, but occurred some little slight cracks, and these little slight cracks can cause material stress to disperse on the one hand under stretching condition, improve the tensile strength of material, but toughness but reduce relatively; On the other hand, the water-absorbent of a little crackle to material does not also have a significant impact.
(1) factor affecting cottonseed protein extraction yield mainly contains the pH value of extraction liquid, temperature, time and liquid pool ratio.Wherein, the influence factor of liquid pool ratio is little.The pH value adjusted when acid is 4.8, and the pH value that alkali is adjusted is 11, and temperature is 50 DEG C, has maximum extracted rate when the time is 70min clock.
(2) plasticization effect of glycerine to plastics with cotton seed protein is obvious.Along with the increase of glycerol content, the tensile strength of plastics with cotton seed protein reduces, and elongation at break increases, and water regain increases obviously.When glycerol content is 20% of cottonseed protein content, there is best plasticization effect.Now, tensile strength reduces less, and elongation at break increase is added, and is beneficial to processing, and little to the performance impact of plastics with cotton seed protein itself.According to processibility and mechanical property Comprehensive Correlation, glycerine number should select 20 parts/100 parts cottonseed proteins.
(3) glutaraldehyde cross-linking cottonseed protein plastics have better mechanical property than textile seed protein plastic, and effectively reduce its water-absorbent.In preparation process glutaraldehyde content and molding temperature remarkable to its Effect on Mechanical Properties.When glutaraldehyde content increases progressively, tensile strength has just started to increase obviously, and then tend towards stability gradually, elongation at break declines rapidly, finally also tends towards stability; Water absorbing properties is but first decline rapidly, then tend towards stability.When glutaraldehyde content is cottonseed protein quality 30%, when molding temperature is 140 DEG C, the tensile strength of cottonseed protein plastics reaches 17.22MPa, and water-intake rate is also down to 44.8%.The optimum proportioning of glutaraldehyde modification cottonseed protein plastics is cottonseed protein 100 parts, glutaraldehyde 30 parts.
(4) plastics with cotton seed protein of montmorillonite intercalation glutaraldehyde cross-linking has optimum mechanical property, along with the increase of polynite content, the tensile strength of plastics with cotton seed protein increases sharply, and slowly decline after arriving some strength, elongation at break is in downtrending always again; Water absorbing properties presents the trend that first increasing declines again increases again.When polynite content is 6%, tensile strength is the highest, and be 19.1MPa, water-intake rate is minimum, is 27.8%.Comprehensive Correlation, polynite number should select 6 parts/100 parts cottonseed protein the bests.
Claims (4)
1. a preparation method for cottonseed protein degradative plastics, is characterized in that, described method comprises following process:
First, the extraction of cottonseed protein, select the grouts after cottonseed oil expression of peeling off, pulverize with pulverizer, sieve, getting powder is raw material, treats that next step uses after drying; Take cottonseed meal, measure distilled water, add sodium hydroxide, in a water bath heated and stirred; Extract complete, centrifugation, get supernatant liquid and treat that next step uses; Supernatant liquor hydrochloric acid soln carries out titration, is titrated to the pH value needed for test, stops acid adding, carries out centrifugation, get precipitation, with deionized water wash, be put in air dry oven and carry out drying, obtain cottonseed protein isolate; Then finished product is prepared step by step as follows:
(1) cottonseed protein/glycerine is prepared: by cottonseed protein, add glycerine, dispersed with stirring; This mixture is imported culture dish, dries in vacuum drying oven;
Sample after drying is molded into sheet on vulcanizing press, then moves in another normal temperature press and cool; Leave standstill in atmosphere after print is cut into test bars, test its properties;
(2) cottonseed protein/glycerine/glutaraldehyde is prepared: after preparing cottonseed protein/glycerol mixture with (1), then add glutaraldehyde, react in hot water bath, add glutaraldehyde; Subsequent process is with method for making sample is consistent above;
(3) cottonseed protein/glycerine/glutaraldehyde/sodium-based montmorillonite is prepared: in (2), add the polynite solution of purifying through quiet settling process in preparation, fully mix, add polynite, subsequent process is with method for making sample is consistent above.
2. the preparation method of a kind of cottonseed protein degradative plastics according to claim 1, is characterized in that, described glycerine number selects 20 parts/100 parts cottonseed proteins to be good.
3. the preparation method of a kind of cottonseed protein degradative plastics according to claim 1, it is characterized in that, described glutaraldehyde content is 30% of cottonseed protein quality, when molding temperature is 140 DEG C, the tensile strength of cottonseed protein plastics reaches 17.22MPa, and water-intake rate is also down to 44.8%; The optimum proportioning of glutaraldehyde modification cottonseed protein plastics is cottonseed protein 100 parts, glutaraldehyde 30 parts.
4. the preparation method of a kind of cottonseed protein degradative plastics according to claim 1, is characterized in that, when described polynite content is 6%, tensile strength is the highest, and be 19.1MPa, water-intake rate is minimum, is 27.8%; Comprehensive Correlation, polynite number should select 6 parts/100 parts cottonseed protein the bests.
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| CN113308122A (en) * | 2021-06-03 | 2021-08-27 | 清华大学 | Degradable protein plastic and preparation method thereof |
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| CN101747634A (en) * | 2009-12-11 | 2010-06-23 | 沈阳化工学院 | Method for preparing plastics with cotton seed protein |
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| US20050191390A1 (en) * | 2004-03-01 | 2005-09-01 | The Regents Of The University Of California | Methods and formulations for providing gloss coatings to foods and for protecting nuts from rancidity |
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Cited By (3)
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| CN110591390A (en) * | 2019-09-19 | 2019-12-20 | 广东工业大学 | Dialdehyde starch crosslinked fiber/cottonseed protein composite material and preparation method and application thereof |
| CN110591390B (en) * | 2019-09-19 | 2021-09-17 | 广东工业大学 | Dialdehyde starch crosslinked fiber/cottonseed protein composite material and preparation method and application thereof |
| CN113308122A (en) * | 2021-06-03 | 2021-08-27 | 清华大学 | Degradable protein plastic and preparation method thereof |
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Application publication date: 20160210 |