CN114573878A - Preparation method and application of food-medicine grade biological cellulose transparent material - Google Patents
Preparation method and application of food-medicine grade biological cellulose transparent material Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/287—Calcium, strontium or barium nitrates
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- C08K3/32—Phosphorus-containing compounds
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- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a preparation method and application of a food-medicine grade biological cellulose transparent material, belonging to the field of polysaccharide and derivatives thereof. The cellulose transparent material has high transparency and high haze, wherein the transparency is 88-89%, and the haze is 89-91%; low thermal expansion coefficient of 2.8-2.9X 10−6/℃。
Description
Technical Field
The invention relates to a preparation method and application of a food-medicine grade biological cellulose transparent material, belonging to the field of polysaccharide and derivatives thereof.
Background
Cellulose is a natural polysaccharide with the largest storage capacity and the widest distribution in nature, is widely applied to the aspects of paper, building materials, furniture, fabrics and the like, and has important strategic significance in paying attention to the development of renewable cellulose polysaccharide resources under the situations of rapid resource consumption and environmental deterioration in the world nowadays.
The cellulose material prepared by the general method has insufficient transparency, cannot provide a material with ultrahigh light transmittance, and has narrow application range; at present, the transparency of cellulose materials can be improved in the prior art, but the transparency is improved, the haze is low, the scattering performance of incident light is poor, and the application of the cellulose materials is limited. CN107922509A discloses a method for preparing a cellulose-based material, which belongs to the field of polysaccharide and derivatives thereof, wherein a bleaching agent is used for preparing a transparent cellulose solution in the film production process, and then a film material is prepared, so that a cellulose film material with high transparency is finally obtained, but the haze is low, and the scattering effect on incident light is poor.
CN110552233B discloses a paper-based transparent material, a preparation method and an application thereof, the obtained paper-based transparent material has the characteristic of high transparency, and also has the problems of low haze, poor light scattering performance, high thermal expansion coefficient, and influence on other performances due to certain expansion under the condition of temperature rise.
In summary, the prior art has the following disadvantages:
(1) the haze of the existing cellulose material is reduced while the transparency is improved, and the haze of the material cannot be improved;
(2) the existing cellulose material has high thermal expansion coefficient.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art, and realizes the following purposes by mixing and blasting dry meal and modified nano ceramic powder, modifying blasting materials and preparing a cellulose transparent material:
(1) the transparency of the cellulose material is improved, and the haze of the material is improved;
(2) the cellulose material has a low coefficient of thermal expansion.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a food-medicine grade biological cellulose transparent material comprises the steps of boiling pulp, blasting dry meal, modifying blasting materials and preparing membranes;
the following is a further improvement of the above technical solution:
the pulp boiling comprises the steps of mixing cotton pulp and pine pulp to obtain mixed pulp, adding sodium hydroxide and sodium sulfite, boiling for 80-120min, filtering, adding sodium hypochlorite solution into filter residues, stirring for 50-90min at 50-70 ℃, filtering, washing and drying to obtain dry pulp.
The mass ratio of the cotton pulp to the pine pulp is 2.5-3.5: 1;
the solid content of the cotton pulp is 25-35%;
the solid content of the pine pulp is 45-55%;
the mass ratio of the sodium hydroxide to the mixed pulp is 1: 4-6;
the mass ratio of the sodium sulfite to the mixed pulp is 1: 12-17;
the mass ratio of the filter residue to the sodium hypochlorite solution is 1: 2.5-3.5;
the effective chlorine content of the sodium hypochlorite solution is 2.5-3.5 g/L.
The dry meal blasting is to mix the dry meal, sodium hydroxide solution and modified nano ceramic powder and put the mixture into a steam blasting tank, the temperature is 130-150 ℃, the pressure is maintained at 1.0-1.3Mpa for 20-30min, the pressure is relieved for blasting, and the blasting material is obtained after filtration, cleaning and drying;
the mass ratio of the dry meal, the sodium hydroxide solution and the modified nano ceramic powder is 18-22:13-17: 1;
the mass concentration of the sodium hydroxide solution is 8-12%.
Dispersing the nano ceramic powder in an ethanol solution, adjusting the pH value to 5.3-6.0 by hydrochloric acid, adding gamma-mercaptopropyltriethoxysilane, stirring at 40-60 ℃ for 50-90min, heating to 70-90 ℃ for 20-40min, keeping for 50-90min, filtering, drying, and keeping for 1.5-2.5h under vacuum at 100-110 ℃ to obtain modified nano ceramic powder;
the mass ratio of the nano ceramic powder to the ethanol solution is 1: 15-25;
the mass concentration of the ethanol solution is 80-95%;
the mass ratio of the gamma-mercaptopropyltriethoxysilane to the nano ceramic powder is 1: 25-35.
And the blasting material is modified, the blasting material is mixed with hydrochloric acid solution, ferric sodium pyrophosphate, potassium polymetaphosphate and calcium nitrate are added, the mixture is heated to 50-60 ℃ under 0.30-0.40Mpa, stirred for 320-380min, filtered, cleaned and dried to obtain the modified blasting material.
The mass ratio of the blasting material to the hydrochloric acid solution is 1: 2.5-3.5;
the mass concentration of the hydrochloric acid solution is 30-50%;
the mass ratio of the ferric sodium pyrophosphate to the blasting material is 1: 6-8;
the mass ratio of the potassium polymetaphosphate to the blasting material is 1: 9-12;
the mass ratio of the calcium nitrate to the blasting material is 1: 4.5-5.5.
The method comprises the steps of preparing a membrane, namely humidifying the modified blasting material until the water content is 20-30%, and performing thermosetting pressing at 8-12Mpa for 15-25min to obtain the cellulose transparent material.
The prepared food-medicine grade biological cellulose transparent material can be applied to food-medicine packaging.
Compared with the prior art, the invention has the following beneficial effects:
the cellulose transparent material has high transparency and high haze, wherein the transparency is 88-89%, and the haze is 89-91%;
the cellulose transparent material of the invention has low thermal expansion coefficient which is 2.8-2.9 multiplied by 10−6/℃；
The cellulose transparent material has high strength, and the tensile strength is 124-127 MPa;
the cellulose transparent material has good hydrophobicity, and the contact angle of the cellulose transparent material with water is 96-98 degrees.
Detailed Description
Example 1
(1) Boiling milk
Mixing cotton pulp and pine pulp to obtain mixed pulp, adding sodium hydroxide and sodium sulfite, boiling and heating for 90min, filtering after heating, adding sodium hypochlorite solution into filter residue, stirring for 60min at 60 ℃, filtering again, washing filter residue and drying to obtain dry pulp;
the mass ratio of the cotton pulp to the pine pulp is 3: 1;
the solid content of the cotton pulp is 30 percent;
the solid content of the pine pulp is 50 percent;
the mass ratio of the sodium hydroxide to the mixed pulp is 1: 5;
the mass ratio of the sodium sulfite to the mixed pulp is 1: 15;
the mass ratio of the filter residue to the sodium hypochlorite solution is 1: 3;
the effective chlorine content of the sodium hypochlorite solution is 3 g/L.
(2) Blasting of dry meal
Mixing the dry meal, a sodium hydroxide solution and the modified nano ceramic powder, putting the mixture into a steam explosion tank, maintaining the temperature at 140 ℃ under the pressure of 1.2Mpa for 25min, then carrying out pressure relief explosion, filtering, cleaning and drying to obtain a blasting material, and detecting that the content of lignin in the blasting material is 0.23%;
the mass ratio of the dry meal to the sodium hydroxide solution to the modified nano ceramic powder is 20:15: 1;
the mass concentration of the sodium hydroxide solution is 10 percent;
dispersing the nano ceramic powder in an ethanol solution, adjusting the pH to 5.6 by hydrochloric acid, adding gamma-mercaptopropyltriethoxysilane, stirring for 60min at 50 ℃, heating to 80 ℃ for 60min after 30min, keeping for 60min, filtering, drying, and keeping for 2h at 105 ℃ under vacuum to obtain modified nano ceramic powder;
the mass ratio of the nano ceramic powder to the ethanol solution is 1: 20;
the mass concentration of the ethanol solution is 90 percent;
the mass ratio of the gamma-mercaptopropyltriethoxysilane to the nano ceramic powder is 1: 30.
(3) Modification of blasting materials
Mixing the blasting material with hydrochloric acid solution, adding sodium ferric pyrophosphate, potassium polymetaphosphate and calcium nitrate, heating to 55 deg.C under 0.35Mpa, stirring for 350min, filtering, cleaning and drying to obtain modified blasting material;
the mass ratio of the blasting material to the hydrochloric acid solution is 1: 3;
the mass concentration of the hydrochloric acid solution is 40%;
the mass ratio of the ferric sodium pyrophosphate to the blasting material is 1: 7;
the mass ratio of the potassium polymetaphosphate to the blasting material is 1: 10;
the mass ratio of the calcium nitrate to the blasting material is 1:5.
(4) Film production
Spraying water on the modified blasting material until the water content is 25%, and performing hot curing pressing at 10Mpa for 20min to obtain a cellulose transparent material;
the cellulose transparent material can be used for packaging food and medicine.
The cellulose transparent material of the embodiment 1 has high transparency and high haze, wherein the transparency is 89 percent and the haze is 91 percent;
the cellulose transparent material of example 1 had a low coefficient of thermal expansion of 2.8X 10−6/℃；
The cellulose transparent material of example 1 has high strength, and the tensile strength is 127 Mpa;
the cellulose transparent material of example 1 had good hydrophobicity and a contact angle with water of 98 °.
Example 2
(1) Boiling milk
Mixing cotton pulp and pine pulp to obtain mixed pulp, adding sodium hydroxide and sodium sulfite, boiling and heating for 80min, filtering after heating, adding sodium hypochlorite solution into the filter residue, stirring for 90min at 50 ℃, filtering again, washing the filter residue and drying to obtain dry pulp;
the mass ratio of the cotton pulp to the pine pulp is 2.5: 1;
the solid content of the cotton pulp is 25 percent;
the solid content of the pine pulp is 55 percent;
the mass ratio of the sodium hydroxide to the mixed pulp is 1: 4;
the mass ratio of the sodium sulfite to the mixed pulp is 1: 12;
the mass ratio of the filter residue to the sodium hypochlorite solution is 1: 2.5;
the effective chlorine content of the sodium hypochlorite solution is 2.5 g/L.
(2) Blasting of dry meal
Mixing the dry meal, a sodium hydroxide solution and the modified nano ceramic powder, putting the mixture into a steam explosion tank, maintaining the temperature at 130 ℃ under the pressure of 1.3Mpa for 20min, then carrying out pressure relief explosion, filtering, cleaning and drying to obtain a blasting material, and detecting that the content of lignin in the blasting material is 0.24%;
the mass ratio of the dry meal to the sodium hydroxide solution to the modified nano ceramic powder is 18:13: 1;
the mass concentration of the sodium hydroxide solution is 8%;
dispersing the nano ceramic powder in an ethanol solution, adjusting the pH to 5.3 by hydrochloric acid, adding gamma-mercaptopropyltriethoxysilane, stirring for 90min at 40 ℃, heating to 70 ℃ for 90min after 20min, keeping for 90min, filtering, drying, and keeping for 2.5h at 100 ℃ under vacuum to obtain modified nano ceramic powder;
the mass ratio of the nano ceramic powder to the ethanol solution is 1: 15;
the mass concentration of the ethanol solution is 80%;
the mass ratio of the gamma-mercaptopropyltriethoxysilane to the nano-ceramic powder is 1: 25.
(3) Modification of blasting materials
Mixing the blasting material with hydrochloric acid solution, adding sodium ferric pyrophosphate, potassium polymetaphosphate and calcium nitrate, heating to 60 deg.C under 0.30Mpa, stirring for 380min, filtering, cleaning and drying to obtain modified blasting material;
the mass ratio of the blasting material to the hydrochloric acid solution is 1: 2.5;
the mass concentration of the hydrochloric acid solution is 50%;
the mass ratio of the ferric sodium pyrophosphate to the blasting material is 1: 6;
the mass ratio of the potassium polymetaphosphate to the blasting material is 1: 9;
the mass ratio of the calcium nitrate to the blasting material is 1: 4.5.
(4) Film production
Spraying water on the modified blasting material until the water content is 20%, and performing thermal curing pressing at 8Mpa for 25min to obtain a cellulose transparent material;
the cellulose transparent material can be used for packaging food and medicine.
The cellulose transparent material of the embodiment 2 has high transparency and high haze, wherein the transparency is 88 percent, and the haze is 90 percent;
the cellulose transparent material of example 2 had a low coefficient of thermal expansion of 2.9X 10−6/℃；
The cellulose transparent material of example 2 has high strength, and the tensile strength is 126 Mpa;
the cellulose transparent material of example 2 had good hydrophobicity with a contact angle with water of 96 °.
Example 3
(1) Boiling milk
Mixing cotton pulp and pine pulp to obtain mixed pulp, adding sodium hydroxide and sodium sulfite, boiling and heating for 120min, filtering after heating, adding sodium hypochlorite solution into filter residue, stirring for 50min at 70 ℃, filtering again, washing filter residue and drying to obtain dry pulp;
the mass ratio of the cotton pulp to the pine pulp is 3.5: 1;
the solid content of the cotton pulp is 35 percent;
the solid content of the pine pulp is 45 percent;
the mass ratio of the sodium hydroxide to the mixed pulp is 1: 6;
the mass ratio of the sodium sulfite to the mixed pulp is 1: 17;
the mass ratio of the filter residue to the sodium hypochlorite solution is 1: 3.5;
the effective chlorine content of the sodium hypochlorite solution is 3.5 g/L.
(2) Blasting of dry meal
Mixing the dry meal, a sodium hydroxide solution and the modified nano ceramic powder, putting the mixture into a steam explosion tank, maintaining the temperature at 150 ℃ under the pressure of 1.0Mpa for 30min, then carrying out pressure relief explosion, filtering, cleaning and drying to obtain a blasting material, and detecting that the content of lignin in the blasting material is 0.22%;
the mass ratio of the dry meal to the sodium hydroxide solution to the modified nano ceramic powder is 22:17: 1;
the mass concentration of the sodium hydroxide solution is 12%;
dispersing the nano ceramic powder in an ethanol solution, adjusting the pH to 6.0 by hydrochloric acid, adding gamma-mercaptopropyltriethoxysilane at 60 ℃, stirring for 50min, heating to 90 ℃ for 40min, keeping for 50min, filtering, drying, and keeping for 1.5h at 110 ℃ under vacuum to obtain modified nano ceramic powder;
the mass ratio of the nano ceramic powder to the ethanol solution is 1: 25;
the mass concentration of the ethanol solution is 95 percent;
the mass ratio of the gamma-mercaptopropyltriethoxysilane to the nano ceramic powder is 1: 35.
(3) Modification of blasting material
Mixing the blasting material with a hydrochloric acid solution, adding sodium ferric pyrophosphate, potassium polymetaphosphate and calcium nitrate, heating to 50 ℃ under 0.40Mpa, stirring for 320min, filtering, cleaning and drying to obtain a modified blasting material;
the mass ratio of the blasting material to the hydrochloric acid solution is 1: 3.5;
the mass concentration of the hydrochloric acid solution is 30%;
the mass ratio of the ferric sodium pyrophosphate to the blasting material is 1: 8;
the mass ratio of the potassium polymetaphosphate to the blasting material is 1: 12;
the mass ratio of the calcium nitrate to the blasting material is 1: 5.5.
(4) Film production
Spraying water to the modified blasting material until the water content is 30%, and performing hot curing pressing at 12Mpa for 15min to obtain a cellulose transparent material;
the cellulose transparent material can be used for packaging food and medicine.
The cellulose transparent material of example 3 has high transparency and high haze, the transparency is 88% and the haze is 89%;
the cellulose transparent material of example 3 had a low coefficient of thermal expansion of 2.8X 10−6/℃；
The cellulose transparent material of example 3 has high strength, and the tensile strength is 124 Mpa;
the cellulose transparent material of example 3 had good hydrophobicity and a contact angle with water of 97 °.
Comparative example 1
On the basis of the embodiment 1, the dry meal blasting step is omitted, the dry meal is directly mixed with a sodium hydroxide solution and modified nano ceramic powder, the mixture is stirred for 60min at the temperature of 40 ℃, then the mixture is filtered, cleaned and dried, and then the filter residue is modified according to the same method as the method for modifying the blasting material in the step (3) to obtain modified filter residue, and the modified filter residue is used for preparing a cellulose material according to the same method for preparing the membrane in the step (4);
the mass ratio of the dry meal to the sodium hydroxide solution to the modified nano ceramic powder is 20:15: 1;
the cellulose material of comparative example 1 had a transparency of 70% and a haze of 65%;
the cellulose material of comparative example 1 had a thermal expansion coefficient of 3.7X 10−6/℃；
The tensile strength of the cellulosic material of comparative example 1 was 112 Mpa;
the cellulose material of comparative example 1 had a contact angle with water of 91 °.
Comparative example 2
On the basis of the embodiment 1, in the dry meal blasting step, the addition of modified nano ceramic powder is omitted, the dry meal, sodium hydroxide solution and unmodified nano ceramic powder are mixed and put into a steam blasting tank for steam blasting, and the other steps are the same, so that the cellulose material is prepared;
the mass ratio of the dry meal to the sodium hydroxide solution to the unmodified nano ceramic powder is 20:15: 1;
the cellulose material of comparative example 2 had a transparency of 77% and a haze of 72%;
the cellulose material of comparative example 2 had a thermal expansion coefficient of 5.2X 10−6/℃；
The tensile strength of the cellulosic material of comparative example 2 was 97 Mpa;
the contact angle with water of the cellulose material of comparative example 2 was 82 °.
Comparative example 3
On the basis of the embodiment 1, a blasting material modification step is omitted, the blasting material obtained in the step (2) is directly used for preparing the cellulose material according to the same method as the film preparation step in the step (4), and the rest steps are the same;
the cellulosic material of comparative example 3 had a transparency of 75% and a haze of 63%;
the cellulose material of comparative example 3 had a thermal expansion coefficient of 4.5X 10−6/℃；
The tensile strength of the cellulosic material of comparative example 3 was 120 Mpa;
the contact angle with water of the cellulose material of comparative example 3 was 85 °.
Claims (6)
1. A preparation method of a food-medicine grade biological cellulose transparent material is characterized by comprising the steps of boiling pulp, blasting dry meal, modifying blasting materials and preparing a membrane;
the dry meal blasting is to mix the dry meal, sodium hydroxide solution and modified nano ceramic powder and put the mixture into a steam blasting tank, the temperature is 130-150 ℃, the pressure is maintained at 1.0-1.3Mpa for 20-30min, the pressure is relieved for blasting, and the blasting material is obtained after filtration, cleaning and drying;
dispersing the nano ceramic powder in an ethanol solution, adjusting the pH value to 5.3-6.0 by hydrochloric acid, adding gamma-mercaptopropyltriethoxysilane, stirring at 40-60 ℃ for 50-90min, heating to 70-90 ℃ for 20-40min, keeping the temperature for 50-90min, filtering and drying to obtain modified nano ceramic powder;
and the blasting material is modified, the blasting material is mixed with hydrochloric acid solution, ferric sodium pyrophosphate, potassium polymetaphosphate and calcium nitrate are added, the mixture is heated to 50-60 ℃ under 0.30-0.40Mpa, stirred for 320-380min, filtered, cleaned and dried to obtain the modified blasting material.
2. The method for preparing a food-pharmaceutical grade bio-cellulose transparent material according to claim 1, wherein the method comprises the following steps:
the mass ratio of the dry meal, the sodium hydroxide solution and the modified nano ceramic powder is 18-22:13-17: 1;
the mass concentration of the sodium hydroxide solution is 8-12%;
the mass ratio of the nano ceramic powder to the ethanol solution is 1: 15-25;
the mass concentration of the ethanol solution is 80-95%;
the mass ratio of the gamma-mercaptopropyltriethoxysilane to the nano-ceramic powder is 1: 25-35;
the mass ratio of the blasting material to the hydrochloric acid solution is 1: 2.5-3.5;
the mass concentration of the hydrochloric acid solution is 30-50%;
the mass ratio of the ferric sodium pyrophosphate to the blasting material is 1: 6-8;
the mass ratio of the potassium polymetaphosphate to the blasting material is 1: 9-12;
the mass ratio of the calcium nitrate to the blasting material is 1: 4.5-5.5.
3. The method for preparing a food-pharmaceutical grade bio-cellulose transparent material according to claim 1, wherein the method comprises the following steps:
the pulp boiling comprises the steps of mixing cotton pulp and pine pulp into mixed pulp, adding sodium hydroxide and sodium sulfite, boiling for 80-120min, filtering, adding sodium hypochlorite solution into filter residues, stirring for 50-90min, filtering, washing and drying to obtain dry pulp.
4. The method for preparing a food-pharmaceutical grade bio-cellulose transparent material according to claim 3, wherein:
the mass ratio of the cotton pulp to the pine pulp is 2.5-3.5: 1;
the solid content of the cotton pulp is 25-35%;
the solid content of the pine pulp is 45-55%;
the mass ratio of the sodium hydroxide to the mixed pulp is 1: 4-6;
the mass ratio of the sodium sulfite to the mixed pulp is 1: 12-17;
the mass ratio of the filter residue to the sodium hypochlorite solution is 1: 2.5-3.5;
the effective chlorine content of the sodium hypochlorite solution is 2.5-3.5 g/L.
5. The method for preparing a food-pharmaceutical grade bio-cellulose transparent material according to claim 1, wherein the method comprises the following steps:
and (3) preparing the membrane, namely humidifying the modified blasting material until the water content is 20-30%, and performing thermocuring pressing for 15-25min under the pressure of 8-12Mpa to obtain the cellulose transparent material.
6. Use of a food-and-medicine grade transparent material of bio-cellulose prepared according to claim 1 in food-and-medicine packaging.
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