CN107793578B - Glutinous rice pulp-bone glue composite gel material, preparation method and application thereof - Google Patents

Glutinous rice pulp-bone glue composite gel material, preparation method and application thereof Download PDF

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CN107793578B
CN107793578B CN201610787010.3A CN201610787010A CN107793578B CN 107793578 B CN107793578 B CN 107793578B CN 201610787010 A CN201610787010 A CN 201610787010A CN 107793578 B CN107793578 B CN 107793578B
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glutinous rice
bone glue
gel material
composite gel
weight
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CN107793578A (en
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方世壁
胡涛
张洪磊
张志龄
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BEIJING UNION - ENGINEERING TRADE CENTER
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L3/00Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
    • C08L3/02Starch; Degradation products thereof, e.g. dextrin
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2303/00Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
    • C08J2303/02Starch; Degradation products thereof, e.g. dextrin
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2489/00Characterised by the use of proteins; Derivatives thereof

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Cereal-Derived Products (AREA)

Abstract

The invention provides a glutinous rice paste-bone glue composite gel material, a preparation method and application thereof. The preparation method comprises the following steps: (1) mixing glutinous rice, water, alum and sodium hydroxide to obtain glutinous rice pulp; (2) contacting the glutinous rice pulp, the bone glue, the sodium hydroxide aqueous solution, the epichlorohydrin and the hydrochloric acid so as to obtain the glutinous rice pulp-bone glue composite gel material. The preparation method provided by the invention can prepare the composite gel material with high mechanical property, high durability or good frost resistance, saves energy, has low processing degree and is environment-friendly, and through compounding the glutinous rice pulp and the bone glue, the durability of the composite gel material is improved, and meanwhile, the composite gel material is in a liquid state at normal temperature, thereby being beneficial to the simplicity and convenience of operations such as coating, mechanical glue application and the like.

Description

Glutinous rice pulp-bone glue composite gel material, preparation method and application thereof
Technical Field
The invention relates to the field of earthen site protection engineering and civil engineering, in particular to a glutinous rice paste-bone glue composite gel material, a preparation method and application thereof.
Background
Ancient buildings are becoming extinct at an alarming rate due to natural efflorescence and artificial destruction, and industrial development and urbanization bring a large amount of chemical byproducts. With the responsibility of ancient architecture restoration to the whole society and the increasingly urgent social requirements of environment-friendly and environment-friendly ancient architectures, an environment-friendly ancient architecture cultural relic reinforced cementitious material is needed. Glutinous rice paste and bone glue are all intelligent crystals left in the historical long river of China, and no volatile organic solvent escapes in the using process.
At present, the research on environment-friendly gel materials is still in need of development.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
The present invention has been completed based on the following findings of the inventors:
the inventor finds that the preparation of the pure glutinous rice pulp does not involve high-molecular polymerization reaction, but the strength of the pure glutinous rice pulp is mainly derived from inorganic reaction which can occur when the glutinous rice pulp and the pseudo-ginseng ash are mixed and then contact with air in subsequent treatment, and stress enhancement points such as calcium carbonate, ettringite and the like which can increase the body strength are generated. Although such a blend system can improve the mechanical strength of the matrix, it does not exhibit the desired effects of water resistance and freeze-thaw cycle resistance.
The inventor further researches and discovers that the bone glue as a high molecular material of amino acids has remarkable advantages in enhancing and improving the freezing resistance. Therefore, in the glutinous rice slurry added with the bone glue, the carboxyl of the bone glue molecules and the hydroxyl of the glutinous rice molecules can generate esterification reaction, so that the strength and the durability of the composite gel material can be improved; and the amino group of the bone glue molecule can destroy the hydrogen bond function among the bone glue molecules under the substitution effect of the modifier epichlorohydrin, so that the freezing point of the composite gel material is reduced, and the composite gel material still keeps liquid state at normal temperature. The compounded glutinous rice pulp-bone glue composite gel material is non-toxic and harmless, is in a liquid state at normal temperature, has high mechanical strength and obviously improves the durability; and the combination of the two substances can also solve the problems of low mechanical strength and weak durability of the single glutinous rice paste.
In view of the above, an object of the present invention is to provide a method for preparing a glutinous rice slurry-bone glue composite gel material with high mechanical strength, high durability, environmental friendliness or energy saving.
In a first aspect of the present invention, the present invention provides a method for preparing a glutinous rice slurry-bone glue composite gel material.
According to an embodiment of the invention, the method comprises: (1) mixing glutinous rice, water, alum and sodium hydroxide to obtain glutinous rice pulp; (2) and contacting the glutinous rice pulp, the bone glue, the sodium hydroxide aqueous solution, the epichlorohydrin and the hydrochloric acid to obtain the glutinous rice pulp-bone glue composite gel material.
The invention has the advantages that the preparation method provided by the embodiment of the invention can be used for preparing the composite gel material with high mechanical property, high durability or good frost resistance, the method is energy-saving, low in processing degree and environment-friendly, the durability of the composite gel material is improved by compounding the glutinous rice pulp and the bone glue, and the liquid state at normal temperature is beneficial to the simplicity of operations such as coating, mechanical sizing and the like.
In addition, the preparation method according to the above embodiment of the present invention may further have the following additional technical features:
according to the embodiment of the invention, in the step (1), the weight ratio of the glutinous rice, the water, the alum and the sodium hydroxide is (10-15): (90-110): (0.4-0.8): (0.1 to 0.3); and the mixing is carried out at a temperature of 60-90 ℃, and the mixing time is 1-4 hours. The inventor researches and discovers that the glutinous rice pulp has wide sources of raw materials for preparing the glutinous rice pulp and low cost, and the weight of the added alum and the sodium hydroxide aqueous solution can be finely adjusted according to the proportion of the glutinous rice and the water; the mixing effect is optimal when the temperature is 60-90 ℃, the starch in the sticky rice cannot be gelatinized and cannot be dissolved in water when the temperature is lower than 60 ℃, and the starch in the sticky rice starts to be thermally decomposed when the temperature is higher than 90 ℃; the mixing time is too short or too long, which is not beneficial to the gelatinization effect of the glutinous rice pulp, so that the next chemical reaction can be influenced.
Therefore, the preparation method of the glutinous rice paste is simple and convenient, mild in condition and short in reaction time, and the glutinous rice is gelatinized by the alum and the sodium hydroxide aqueous solution to completely destroy all glutinous rice micelle molecules, so that the solubility and the dispersibility of starch single molecules in the glutinous rice paste in the aqueous solution are improved, and the glutinous rice paste which is beneficial to further carrying out chemical reaction with bone glue is obtained.
According to the embodiment of the invention, the step (2) is specifically as follows: adding bone glue into the glutinous rice pulp for heating and dissolving, adding a sodium hydroxide aqueous solution for degradation, adding epichlorohydrin for crosslinking, and adding hydrochloric acid for esterification to obtain a glutinous rice pulp-bone glue composite gel material; or adding the bone glue into a sodium hydroxide aqueous solution for degradation, adding epichlorohydrin for crosslinking, adding the modified bone glue into the glutinous rice pulp for heating and dissolving, and adding hydrochloric acid for esterification, so as to obtain the glutinous rice pulp-bone glue composite gel material.
The inventor researches and discovers that the terminal amino groups and the terminal carboxyl groups among the bone glue molecules can be mutually associated to form a reticular gel. Therefore, it is necessary to break the gel state of the molecules of the bone glue at normal temperature by heating and adding an alkalizing agent, i.e. an aqueous solution of sodium hydroxide, and to destroy the association between the molecules to release the single molecules of the bone glue. Furthermore, epichlorohydrin is added to perform graft copolymerization with the terminal amino group of the single bone glue molecule to form a modified bone glue molecule with a linear structure, so that the length of the bone glue molecule chain is increased, and the tendency of mutual association among the bone glue molecule chains is reduced. At this time, 1v/v% hydrochloric acid of an esterification catalyst was added to promote an esterification reaction between the terminal carboxyl groups of the modified bone glue molecules and the hydroxyl groups of the single molecules of the glutinous rice starch, thereby obtaining a composite solution containing the glutinous rice pulp-bone glue composite gel material. And finally, cooling the composite solution to normal temperature and filtering to obtain the glutinous rice pulp-bone glue composite gel material. The inventor also finds that the composite gel material with good performance can be obtained by degrading and crosslinking the bone glue in advance and then adding the modified bone glue into the glutinous rice pulp for esterification and composite reaction.
Therefore, the preparation method provided by the embodiment of the invention can be used for preparing the composite gel material with high mechanical property, high durability or good frost resistance, the method is energy-saving, low in processing degree and environment-friendly, the durability of the composite gel material is improved by compounding the glutinous rice pulp and the bone glue, and the liquid state at normal temperature is beneficial to the simplicity of operations such as coating, mechanical sizing and the like.
According to an embodiment of the present invention, in the step (2), the bone glue is used in an amount of 25 parts by weight, and the glutinous rice slurry is used in an amount of 100 to 150 parts by weight. The inventor finds that the proper weight ratio of the bone glue to the glutinous rice pulp is 1: 4-1: 6, too little bone glue is not enough to be completely esterified with starch in the glutinous rice pulp, and too much bone glue can reduce the mechanical property, durability or freezing resistance of the composite gel material. Therefore, by adopting the preparation method provided by the embodiment of the invention, the composite gel material with higher mechanical property, higher durability or better freezing resistance can be prepared by the bone glue and the glutinous rice pulp in a proper weight ratio.
According to an embodiment of the present invention, in step (2), the amount of the aqueous sodium hydroxide solution is 10 parts by weight, the amount of epichlorohydrin is 2 parts by weight, and the amount of hydrochloric acid is 4 parts by weight; wherein the concentration of the sodium hydroxide aqueous solution is 20w/w%, and the concentration of the hydrochloric acid is 1 v/v%. Therefore, by adopting the preparation method provided by the embodiment of the invention, the bone glue is degraded and modified by the sodium hydroxide aqueous solution with specific concentration and the epichlorohydrin, the modified bone glue molecules and starch monomolecular in the glutinous rice paste are subjected to esterification reaction fully under the specific hydrochloric acid concentration, and the glutinous rice paste-bone glue composite gel material with high mechanical property, high durability or high freezing resistance can be formed.
According to the embodiment of the invention, in the step (2), the heating and dissolving are carried out at a temperature of 60-80 ℃, the reaction time of the degradation is 0.5-2 hours, and the heat preservation time of the crosslinking is 0.5-2 hours. The inventor finds that the bone glue has the best dissolution effect at the temperature of 60-90 ℃, so that the dispersibility of the glutinous rice pulp can be maintained, and the release of single molecules of the bone glue can be promoted; the degradation reaction time needs to be 0.5-2 hours, if the reaction time is too short, the bone glue gel is not completely destroyed, and if the reaction time is too long, the degradation of bone glue single molecules is promoted; and the crosslinking heat preservation time is 0.5-2 hours, so that the terminal amino groups of the single molecules of the bone glue are grafted and modified by the epichlorohydrin molecules.
Therefore, by adopting the preparation method provided by the embodiment of the invention, through full degradation, modification and esterification, the glutinous rice pulp-bone glue composite gel material with high mechanical property, high durability or high freezing resistance can be formed, and the method is energy-saving, low in processing degree and environment-friendly.
According to an embodiment of the present invention, the preparation method further comprises: and cooling and filtering the glutinous rice paste-bone glue composite gel material. Therefore, by adopting the preparation method provided by the embodiment of the invention, the glutinous rice paste-bone glue composite gel material with higher purity can be prepared, so that the composite gel material with higher mechanical property, higher durability or better freezing resistance can be obtained.
In a second aspect of the present invention, the present invention provides a method for preparing a glutinous rice pulp-bone glue composite gel material.
According to an embodiment of the invention, the method comprises: (1) mixing 11 parts by weight of glutinous rice with 100 parts by weight of water, adding 0.4 part by weight of alum and 0.2 part by weight of sodium hydroxide, and reacting at 90 ℃ for 1 hour to obtain glutinous rice pulp; (2) adding 25 parts by weight of bone glue into 100 parts by weight of the glutinous rice pulp for dissolving, heating to 80 ℃, adding 10 parts by weight of 20w/w% sodium hydroxide aqueous solution for degradation, reacting for 0.5 hour, adding 2 parts by weight of epichlorohydrin for crosslinking, preserving heat for 1.5 hours, adding 4 parts by weight of 1v/v% hydrochloric acid for esterification, and obtaining a composite solution; (3) and cooling and filtering the composite solution to obtain the glutinous rice pulp-bone glue composite gel material.
The invention has the advantages that the preparation method provided by the embodiment of the invention can be used for preparing the composite gel material with higher mechanical property, higher durability or better frost resistance, the method is energy-saving, low in processing degree and environment-friendly, the durability of the composite gel material is further improved by compounding the glutinous rice pulp and the bone glue, and the liquid state at normal temperature is more beneficial to the simplicity of operations such as coating, mechanical sizing and the like.
In a third aspect of the present invention, the present invention provides a glutinous rice paste-bone glue composite gel material.
According to an embodiment of the present invention, the composite gel material is prepared by the above method.
The inventors surprisingly found that, compared with the traditional glutinous rice paste, the glutinous rice paste-bone glue composite gel material of the embodiment of the invention has high mechanical property, high durability or high frost resistance, is in a liquid state at normal temperature, and is convenient for operations such as coating or mechanical sizing. It will be understood by those skilled in the art that the features and advantages described above with respect to the method for preparing the glutinous rice paste-bone glue composite gel material are still applicable to the glutinous rice paste-bone glue composite gel material, and will not be described herein again.
In a fourth aspect of the invention, the invention provides a use of the glutinous rice paste-bone glue composite gel material in the aspect of repairing ancient architecture cultural relics.
The invention unexpectedly discovers that the glutinous rice paste-bone glue composite gel material disclosed by the embodiment of the invention has high mechanical property, high durability or high frost resistance, is in a liquid state at normal temperature, is convenient to operate such as coating or mechanical sizing and the like, and can be applied to the aspect of ancient cultural relics restoration. It will be understood by those skilled in the art that the features and advantages described above with respect to the glutinous rice paste-bone glue composite gel material are still applicable to the application of the glutinous rice paste-bone glue composite gel material, and will not be described herein again.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
In this example, a glutinous rice slurry, a composite gel material and a sample were prepared in this order according to the following steps.
Firstly, mixing 11g of glutinous rice with 100g of water, adding 0.4g of alum and 0.2g of sodium hydroxide, and reacting at 90 ℃ for 1 hour to obtain glutinous rice pulp;
secondly, adding 25g of bone glue into the decocted glutinous rice pulp 100g for dissolving, heating to 80 ℃, adding 10g of 20w/w% sodium hydroxide aqueous solution for degradation, after reacting for 0.5 hour, dropwise adding 2g of epoxy chloropropane for crosslinking, and after preserving heat for 1.5 hours, adding 4g of 1v/v% hydrochloric acid for esterification to obtain a composite solution;
thirdly, cooling the prepared composite solution, standing for a period of time to room temperature, and filtering to obtain the glutinous rice pulp-bone glue composite gel material;
and step four, weighing the glutinous rice pulp-bone glue composite gel material, and adding the glutinous rice pulp-bone glue composite gel material into the Sanhe soil according to the addition amount of 29 w/w% to prepare a sample.
Example 2
In this example, a glutinous rice slurry and a composite gel material were prepared in substantially the same manner as in example 1.
The difference is that in the first step, 10g of glutinous rice, 110g of water, 0.6g of alum and 0.3g of sodium hydroxide are reacted for 4 hours at 60 ℃; the second step is 125g of glutinous rice pulp, the temperature is raised to 60 ℃, the degradation reaction is carried out for 1 hour, and the crosslinking and heat preservation are carried out for 2 hours; there is no fourth step.
Example 3
In this example, a glutinous rice slurry and a composite gel material were prepared in substantially the same manner as in example 1.
Except that in the first step, 15g of glutinous rice, 90g of water, 0.8g of alum and 0.3 weight percent of sodium hydroxide are reacted for 4 hours at 60 ℃; the second step is 125g of glutinous rice pulp, the temperature is raised to 60 ℃, the degradation reaction is carried out for 4 hours, and the crosslinking and heat preservation are carried out for 4 hours; there is no fourth step.
Example 4
In this example, a glutinous rice slurry and a composite gel material were prepared in substantially the same manner as in example 1.
The difference is that the second step is the modification of bone glue, specifically, 25g of bone glue is mixed with 50g of deionized water, the mixture is dissolved at 60 ℃, the temperature is raised to 80 ℃, 10g of 20w/w% sodium hydroxide aqueous solution is added for degradation, after the reaction is carried out for 0.5 hour, the temperature is reduced to 70 ℃, 2g of epoxy chloropropane is added for crosslinking, and after the temperature is kept for 1.5 hours, the temperature is reduced to obtain the modified bone glue;
thirdly, adding 100g of decocted glutinous rice pulp and 25g of modified bone glue into a reaction kettle, mixing, heating to 80 ℃, and adding 4g of 1v/v% hydrochloric acid for esterification to obtain a composite solution;
and fourthly, cooling the prepared composite solution, standing for a period of time to room temperature, and filtering to obtain the glutinous rice pulp-bone glue composite gel material.
Example 5
In this example, according to substantially the same production method as in example 2, a glutinous rice slurry and a composite gel material were produced.
The difference is that the second step is the modification of bone glue, specifically, 25g of bone glue and 50g of deionized water are mixed, dissolved at 60 ℃, heated to 70 ℃, added with 10g of 20w/w% sodium hydroxide aqueous solution for degradation, reacted for 1 hour, then added with 2g of epoxy chloropropane for crosslinking, and after heat preservation for 2 hours, cooled to obtain the modified bone glue;
thirdly, adding 150g of decocted glutinous rice pulp and 25g of modified bone glue into a reaction kettle, mixing, heating to 80 ℃, and adding 4g of 1v/v% hydrochloric acid for esterification to obtain a composite solution;
and fourthly, cooling the prepared composite solution, standing for a period of time to room temperature, and filtering to obtain the glutinous rice pulp-bone glue composite gel material.
Comparative example 1
In this example, the pure glutinous rice slurry obtained in the first step of example 1 was added to a clay trihydrate in an amount of 29 w/w% to prepare a sample.
Example 6
In this example, the test piece of the glutinous rice paste-bone glue composite gel material-bentonite of example 1 and the test piece of the glutinous rice paste-bentonite of comparative example 1 were subjected to a compression test and a freezing resistance test after 28 days, respectively.
Among them, the compressive strengths of the samples of the 2 groups after being cured for 28 days in an environment of 60% humidity and 20 ℃ were 4.36MPa for the sample of example 1 and 3.18MPa for the sample of comparative example 1, respectively.
The compressive strength of the samples of the group 2 after being maintained in an environment with humidity of 60% and temperature of 20 ℃ for 28 days and then subjected to freeze-thaw cycling for 15 times is respectively reduced by 20% for the sample of example 1, which is 3.48MPa, and 65% for the sample of comparative example 1, which is 1.10 MPa.
Summary of the invention
By combining the embodiments 1-6 and the comparative example 1, the preparation method of the glutinous rice paste-bone glue composite gel material provided by the invention can prepare the composite gel material with high mechanical property, high durability or high frost resistance, the method is energy-saving, low in processing degree and environment-friendly, and the glutinous rice paste and the bone glue are compounded, so that the durability of the composite gel material is improved, and meanwhile, the glutinous rice paste and the bone glue are in a liquid state at normal temperature, and the simplicity of operations such as coating, mechanical glue application and the like is facilitated. Compared with the sample of pure glutinous rice pulp and the sample of the triquetrous soil which are not modified by the bone glue, the sample of the glutinous rice pulp-bone glue composite gel material and the sample of the triquetrous soil have higher compressive strength after 28 days of curing, and the reduction of the compressive strength after 15 times of freeze-thaw cycle is less, which shows that the glutinous rice pulp-bone glue composite gel material has better mechanical property and more excellent freezing resistance.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (9)

1. A method for preparing a glutinous rice paste-bone glue composite gel material is characterized by comprising the following steps:
(1) mixing glutinous rice, water, alum and sodium hydroxide to obtain glutinous rice pulp; and
(2) contacting the glutinous rice pulp, bone glue, a sodium hydroxide aqueous solution, epichlorohydrin and hydrochloric acid to obtain a glutinous rice pulp-bone glue composite gel material;
wherein, step (2) includes:
adding bone glue into the glutinous rice pulp for heating and dissolving, adding a sodium hydroxide aqueous solution for degradation, adding epichlorohydrin for crosslinking, and adding hydrochloric acid for esterification to obtain a glutinous rice pulp-bone glue composite gel material; or
Adding sodium hydroxide aqueous solution into bone glue for degradation, adding epoxy chloropropane for crosslinking, adding the modified bone glue into the glutinous rice pulp for heating and dissolving, and adding hydrochloric acid for esterification so as to obtain the glutinous rice pulp-bone glue composite gel material.
2. The method according to claim 1, wherein, in step (1),
the weight ratio of the glutinous rice, the water, the alum and the sodium hydroxide is (10-15): (90-110): (0.4-0.8): (0.1 to 0.3); and
the mixing is carried out at a temperature of 60-90 ℃, and the mixing time is 1-4 hours.
3. The method according to claim 1, wherein, in step (2),
the amount of bone glue is 25 parts by weight, and
the amount of the glutinous rice slurry is 100 to 150 parts by weight.
4. The method according to claim 1, wherein, in step (2),
the amount of the aqueous sodium hydroxide solution was 10 parts by weight,
the amount of epichlorohydrin is 2 parts by weight, and
the amount of hydrochloric acid is 4 parts by weight;
wherein the concentration of the sodium hydroxide aqueous solution is 20w/w percent, and the concentration of the hydrochloric acid is 1v/v percent.
5. The method according to claim 1, wherein in the step (2), the heating and dissolving are performed at a temperature of 60 to 80 ℃, the reaction time of the degradation is 0.5 to 2 hours, and the holding time of the crosslinking is 0.5 to 2 hours.
6. The method of claim 1, further comprising:
and cooling and filtering the glutinous rice paste-bone glue composite gel material.
7. A method for preparing a glutinous rice paste-bone glue composite gel material is characterized by comprising the following steps:
(1) mixing 11 parts by weight of glutinous rice with 100 parts by weight of water, adding 0.4 part by weight of alum and 0.2 part by weight of sodium hydroxide, and reacting at 90 ℃ for 1 hour to obtain glutinous rice pulp;
(2) adding 25 parts by weight of bone glue into 100 parts by weight of the glutinous rice pulp for dissolving, heating to 80 ℃, adding 10 parts by weight of 20w/w% sodium hydroxide aqueous solution for degradation, reacting for 0.5 hour, adding 2 parts by weight of epichlorohydrin for crosslinking, preserving heat for 1.5 hours, adding 4 parts by weight of 1v/v% hydrochloric acid for esterification, and obtaining a composite solution; and
(3) and cooling and filtering the composite solution to obtain the glutinous rice pulp-bone glue composite gel material.
8. A glutinous rice pulp-bone glue composite gel material, which is prepared by the method according to any one of claims 1 to 7.
9. Use of the glutinous rice pulp-bone glue composite gel material according to claim 8 for repairing ancient architecture cultural relics.
CN201610787010.3A 2016-08-30 2016-08-30 Glutinous rice pulp-bone glue composite gel material, preparation method and application thereof Expired - Fee Related CN107793578B (en)

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CN1840601A (en) * 2005-03-31 2006-10-04 朱寿会 Method for making adhesive made of starch and nontoxic high molecular polymer
CN100519484C (en) * 2007-08-03 2009-07-29 浙江大学 Calcium carbonate biomineralization reinforcing method for calcium carbonate type stone cultural relics
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