CN114796064B - Bagasse calcium phosphate composite material, and preparation method and application thereof - Google Patents

Bagasse calcium phosphate composite material, and preparation method and application thereof Download PDF

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CN114796064B
CN114796064B CN202210630778.5A CN202210630778A CN114796064B CN 114796064 B CN114796064 B CN 114796064B CN 202210630778 A CN202210630778 A CN 202210630778A CN 114796064 B CN114796064 B CN 114796064B
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bagasse
calcium phosphate
composite material
toothpaste
phosphate composite
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CN114796064A (en
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宁科功
高峰
张秋林
郭家文
孔祥烨
蔡英
尚慧
潘波
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Yunnan Baiyao Group Health Products Co ltd
Kunming University of Science and Technology
Institute of Agricultural Environment and Resources of Yunnan Academy of Agricultural Sciences
Sugarcane Research Institute of Yunnan Academy of Agricultural Sciences
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Yunnan Baiyao Group Health Products Co ltd
Kunming University of Science and Technology
Institute of Agricultural Environment and Resources of Yunnan Academy of Agricultural Sciences
Sugarcane Research Institute of Yunnan Academy of Agricultural Sciences
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24Phosphorous; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/02Local antiseptics
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/12Antivirals
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants

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Abstract

The embodiment of the invention discloses a bagasse calcium phosphate composite material, and a preparation method and application thereof. The preparation method comprises the following steps: sequentially carrying out phosphorylation reaction and calcium hydroxide neutralization reaction on bagasse serving as a raw material, and then carrying out centrifugal separation, drying and grinding to obtain the bagasse phosphate calcium composite material. The bagasse calcium phosphate core-shell composite material prepared by taking bagasse as a raw material improves the cleaning performance, elasticity and anti-sensitivity performance of the calcium phosphate abrasive, and keeps excellent biocompatibility.

Description

Bagasse calcium phosphate composite material, and preparation method and application thereof
Technical Field
The embodiment of the invention relates to the technical field of daily chemicals, oral medical treatment, nursing and cleaning products, in particular to a bagasse calcium phosphate composite material, and a preparation method and application thereof.
Background
The calcium phosphate inorganic solid particles and the hydrate thereof are toothpaste abrasive materials with the best taste and biocompatibility, wherein the element compositions of calcium hydrophosphate dihydrate, tricalcium phosphate and hydroxyapatite are similar to the element compositions of enamel surface elements, and the toothpaste prepared by adopting the abrasive materials has unique and fine taste and outstanding performances in aspects of enamel remineralization and dentin anti-sensitivity. However, the production cost of the calcium phosphate inorganic solid particles is relatively high, and the solid particles directly prepared by a precipitation method are large in particle size, so that the cleaning effect of the calcium phosphate inorganic solid particles on tooth gaps is prevented, the calcium phosphate inorganic solid particles are prevented from entering dentinal tubules, and the anti-sensitivity performance of the calcium phosphate abrasive is reduced. In addition, the slightly soluble calcium phosphate inorganic matters can cause eutrophication pollution to water bodies.
Therefore, how to develop an alternative to calcium phosphate-based abrasive and/or tooth desensitizer is a technical challenge in the art.
Disclosure of Invention
Bagasse is a solid organic waste after sugar production of sugarcane, and is commonly used for fuel power generation, papermaking, cellulose extraction, xylitol preparation and the like, and deep processing of bagasse in the processes often causes secondary pollution, so that the requirements of energy conservation, emission reduction and carbon neutralization are difficult to realize.
Bagasse mainly comprises lignin, cellulose and hemicellulose, and is harmless to human body. Lignin has certain antibacterial and antiviral properties, and edible cellulose can help digestion, and hemicellulose polysaccharide is a good prebiotic; the lignin in the bagasse wraps the cellulose and hemicellulose to form a bundle-shaped fiber structure with certain strength; the dried bagasse is easy to absorb water and swell in water at normal temperature, and the volume is increased.
Since Lignin, cellulose, hemicellulose and the like are often connected with each other in nature to form a Lignin-carbohydrate complex (Lignin-Carbohydrate Complex), no method is available at present to separate and obtain original Lignin with completely undamaged structure. Bagasse is considered from a material perspective as a material with a certain mechanical stiffness (lignin) and elasticity (cellulose). Because the molecular structure of lignin has active groups such as aryl, phenolic hydroxyl, alcoholic hydroxyl, carbon-based conjugated double bonds and the like, oxidation, reduction, hydrolysis, alcoholysis, acidolysis, methoxy, carboxyl, photolysis, phthalation, sulfonation, alkylation, halogenation, nitration, polycondensation or graft copolymerization and other chemical reactions can be carried out, and powerful conditions are provided for modifying lignin.
In order to reduce pollution and improve the utilization rate of bagasse, direct modification of bagasse is the most convenient choice. Based on the composition of lignin, cellulose and hemicellulose in bagasse, the selection of hydroxyl end groups contained in all three structures for modification is an ideal choice for maximizing the utilization of bagasse.
In order to reduce the pollution caused by bagasse and calcium phosphate inorganic salt, the cleaning and anti-sensitivity performance of the calcium phosphate toothpaste abrasive is improved, and the excellent biocompatibility is maintained. The invention adopts phosphoric acid to treat the hydroxyl at the bagasse end to prepare the bagasse calcium phosphate core-shell composite material so as to reduce the application amount of inorganic calcium phosphate and reduce the cost, and simultaneously, the bagasse is used as an organic solid waste resource in oral care, and the characteristics of the bagasse needle fiber, such as convenience in deep cleaning of the tooth gaps, are utilized to improve the cleaning performance, the elasticity and the sensitivity resistance of the toothpaste abrasive.
The phosphoric acid is inorganic tribasic acid, and under the condition of adding excessive amount, one hydrogen ion is provided for the terminal hydroxyl group of bagasse, and the other two hydrogen ions react with calcium hydroxide to form a structure of which one end is connected with bagasse and the other end forms calcium phosphate salt, namely bagasse phosphate calcium salt. The bagasse cellulose is wrapped by the bagasse phosphate calcium salt to form a composite material with soft inner core and rigid outer shell, and the material has the characteristics of bundled fibers and good biocompatibility, and can effectively improve the cleaning performance of the toothpaste, block dentin tubules (anti-sensitivity performance), provide good biocompatibility and improve the taste of the toothpaste when applied to the toothpaste.
In order to achieve the above object, the embodiment of the present invention provides the following technical solutions:
according to a first aspect of the embodiment of the invention, the embodiment of the invention provides a preparation method of bagasse calcium phosphate composite material, which comprises the steps of taking bagasse as a raw material, sequentially carrying out a phosphate reaction and a calcium hydroxide neutralization reaction, and then carrying out centrifugal separation, drying and grinding to obtain the bagasse calcium phosphate composite material.
In the invention, the concentration of phosphoric acid used in the phosphorylation reaction is 30% -80%, and the mass ratio of bagasse to phosphoric acid is 1 (3-8).
In the invention, the temperature of the phosphorylation reaction is 70-200 ℃ and the time is 2-4h.
In the present invention, the molar ratio of calcium hydroxide to phosphoric acid is (1 to 1.02): 1.
In the invention, the temperature of the neutralization reaction of the calcium hydroxide is 70-80 ℃ and the time is 0.5-2 h.
In the invention, after the neutralization reaction of the calcium hydroxide is finished, the pH value of the system is regulated to be between 6.75 and 7.50.
In the invention, the grain size of the bagasse calcium phosphate composite material is 0.1-50 microns.
In the invention, the bagasse preparation method comprises the following steps: after sugar is squeezed from sugarcane, water is added for ball milling until the leaching solution is clear and transparent, the leaching solution is sieved by a water sieve with more than 40 meshes, large particles are removed, and the undersize is dried. And jet milling to obtain powder with particle size of 0.1-50 microns
According to a second aspect of embodiments of the present invention, there is provided a bagasse calcium phosphate composite material, which is produced by the production method as described above.
According to a third aspect of embodiments of the present invention, there is provided the use of a bagasse calcium phosphate composite as described above as at least one of an abrasive, an anti-sensitization ingredient in an oral care implement.
In the present invention, the oral care product is a toothpaste, a dentifrice or a tooth desensitizing agent.
According to a fourth aspect of embodiments of the present invention there is provided a toothpaste comprising a bagasse calcium phosphate composite as described above.
In the invention, the bagasse calcium phosphate composite material accounts for 0.1-70% of the toothpaste by mass, and is preferably 10-70%.
In the invention, the toothpaste further comprises at least one of humectant, adhesive, abrasive, essence, preservative, sweetener, foaming agent and water.
Wherein the humectant is humectant conventionally used in the art, such as glycerin, sorbitol, sodium hyaluronate, etc.; the binder is a binder conventionally used in the art, such as xanthan gum, carrageenan, sodium carboxymethyl cellulose, sodium hydroxyethyl cellulose, carbomer, etc.; the abrasive is an abrasive conventionally used in the art, such as calcium carbonate, calcium phosphate salts, silica, and the like; the essence is of a type conventionally used in the art, such as peppermint type, spearmint type, wintergreen type, fruit type, tea type, medicinal type and the like; the preservative is a preservative conventionally used in the art, such as sodium benzoate, parabens, and the like; the sweetener is a sweetener conventionally used in the art, such as sorbitol, xylitol, sodium saccharin, and the like. The foaming agent is a foaming agent conventionally used in the art, such as sodium lauryl sulfate, sodium lauroyl sarcosinate, and the like.
In one embodiment of the present invention, when the toothpaste is abrasive to the bagasse calcium phosphate composite, the toothpaste comprises the following components in weight percent: 1-70% of sorbitol; cellulose gum 0.3-2%; 0.1 to 2 percent of xanthan gum; 0.1 to 2 percent of carrageenan; glycerol 1-50%; 0.1 to 70 percent of bagasse calcium phosphate composite material; essence, preservative, sweetener, foaming agent and water are added in 100%.
In another embodiment of the present invention, when the toothpaste is part of an abrasive material of the bagasse calcium phosphate composite, the toothpaste comprises the following components in weight percent: 15% -80% of humectant (glycerin, sorbitol and mixture thereof in any proportion); 0.4 to 3 percent of adhesive (xanthan gum, carrageenan, sodium carboxymethyl cellulose, hydroxyethyl cellulose sodium, carbomer and any mixture thereof); 7% -60% of abrasive (at least one of calcium carbonate, calcium phosphate and silicon dioxide is included in addition to bagasse calcium phosphate composite material); essence, preservative, sweetener, foaming agent and water are added in 100%.
In yet another embodiment of the present invention, when the bagasse calcium phosphate composite is used as an abrasive and an anti-sensitivity ingredient in a dental anti-sensitivity toothpaste, the dental anti-sensitivity toothpaste comprises the following components in weight percent: 15% -80% of humectant (glycerin, sorbitol and mixture thereof in any proportion); 0.4 to 3 percent of adhesive (xanthan gum, carrageenan, sodium carboxymethyl cellulose, hydroxyethyl cellulose sodium, carbomer and any mixture thereof); 7% -60% of abrasive (at least one of calcium carbonate, calcium phosphate and silicon dioxide is included in addition to bagasse calcium phosphate composite material); potassium nitrate 0.5-7%; essence, preservative, sweetener, foaming agent and water are added in 100%.
The embodiment of the invention has the following advantages:
1. the bagasse calcium phosphate core-shell composite material prepared by taking bagasse as a raw material improves the cleaning performance, elasticity and sensitivity resistance of the calcium phosphate abrasive, and maintains excellent biocompatibility. In addition, the composite material is applied to oral care products, so that the use amount of the calcium phosphate abrasive can be reduced, the cost is reduced, and the pollution caused by calcium phosphate inorganic salts is reduced.
2. The bagasse is applied to the oral care products, so that the anti-inflammatory and antibacterial properties of lignin can be fully exerted, and natural and safe antibacterial and antiviral properties are provided for the oral care products; the carbon neutralization is truly realized, and other toxic chemical substances are not required to be introduced; the carbon captured by the sugarcane from the air is stored in the oral care product for a long time, so that the release period of the carbon is delayed.
3. The preparation method provided by the invention has the advantages of simple and convenient operation of steps, simple process flow, great reduction of cost and contribution to industrial production.
Detailed Description
Other advantages and advantages of the present invention will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The test methods used in the examples are regarded as conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are all commercially available.
Abrasive monocalcium phosphate: particle size 5-150 microns, manufacturer: and (5) creating in the Yunnan Tian.
In the following examples and comparative examples, bagasse was prepared as follows: after sugar is squeezed from sugarcane, 15 times of water is added for 5 times, ball milling is carried out for 3 hours at the rotating speed of 200r/min until the leaching solution is clear and transparent, sieving is carried out through a water sieve with more than 40 meshes, large particles are removed, and the undersize is dried and crushed by air flow, thus obtaining powder with the particle size of 0.1-50 microns.
Example 1
The preparation method of the bagasse calcium phosphate composite material provided by the embodiment comprises the following steps:
1) Weighing 100g of sugarcane slag powder, placing the sugarcane slag powder into a round-bottom flask, adding 400g of phosphoric acid with the concentration of 38%, heating to 90 ℃, and reacting for 4 hours;
2) 114.8g of calcium hydroxide is added, the reaction is carried out for 1h at 80 ℃, and after the reaction is finished, the pH value of the system is regulated to 7.0 by using calcium hydroxide aqueous solution;
3) Centrifuging for 5min at a rotating speed of 1000r/min, drying the obtained solid phase in a drying oven at 105 ℃ for 2h, grinding, and sieving with a 80-mesh sieve to obtain the bagasse calcium phosphate composite material.
Example 2
The preparation method of the bagasse calcium phosphate composite material provided by the embodiment comprises the following steps:
1) Weighing 100g of powder, placing the powder into a round-bottom flask, adding 300g of phosphoric acid with the concentration of 60%, heating to 80 ℃, and reacting for 3 hours;
2) Adding 140g of calcium hydroxide, continuously reacting for 2 hours at 70 ℃, and adjusting the pH value of the system to 7.2 by using a calcium hydroxide aqueous solution after the reaction is finished;
3) Centrifuging for 10min at a rotating speed of 1000r/min, drying the obtained solid in a drying oven at 105 ℃ for 2h, grinding, and sieving with a 100-mesh sieve to obtain the bagasse calcium phosphate composite material.
Example 3
The preparation method of the bagasse calcium phosphate composite material provided by the embodiment comprises the following steps:
1) Weighing 100g of powder, placing the powder into a round-bottom flask, adding 400g of 80% phosphoric acid, heating to 85 ℃, and reacting for 3 hours;
2) 151g of calcium hydroxide is added, the reaction is continued for 3 hours at 90 ℃, and after the reaction is finished, the pH value of the system is regulated to 7.3 by using calcium hydroxide aqueous solution;
3) Centrifuging for 10min at a rotating speed of 1000r/min, drying the obtained solid in a drying oven at 105 ℃ for 3h, grinding, and sieving with a 100-mesh sieve to obtain the bagasse calcium phosphate composite material.
Example 4
The embodiment provides toothpaste, which comprises the following components in percentage by weight:
20% of bagasse calcium phosphate composite material of example 1, 5% of silicon dioxide, 35% of glycerol, 15% of sorbitol, 0.3% of xanthan gum, 0.5% of carrageenan, 0.5% of sodium carboxymethyl cellulose, 1.5% of peppermint essence, 0.5% of sodium benzoate, 0.3% of saccharin sodium, 2% of sodium lauryl sulfate and the balance of water.
The preparation method of the toothpaste comprises the following steps:
1) Adding water, sodium benzoate, saccharin sodium and sorbitol into water phase pot of homogenizing emulsifying equipment, stirring to dissolve;
2) Adding glycerol into an oil phase pot of homogenizing emulsifying equipment, starting stirring at a rotation speed of 100r/min, and adding xanthan gum, carrageenan and sodium carboxymethylcellulose into the oil phase pot until the mixture is uniformly dispersed for later use;
3) Sucking the materials in the oil phase pot into the homogenizing pot through negative pressure, starting wall-mounted stirring (rotating speed of 100 r/min), sucking the materials in the water phase pot into the homogenizing pot through negative pressure, starting homogenizing stirring rotating speed (2000 r/min), stirring for 5min until the materials are uniformly dispersed, and fully swelling;
4) Sucking the bagasse calcium phosphate composite material and silicon dioxide into a homogenizing pot under negative pressure, and stirring for 30 minutes until the system is uniform;
5) Adding peppermint essence into a homogenizing pot, stirring uniformly, and starting vacuum until the negative pressure is less than-0.06 Mp;
6) Sucking sodium laurylsulfate into the homogenizing pot under negative pressure, stirring for 10min, vacuum-starting until negative pressure is less than-0.08 MP, stirring until the system is uniform, and discharging.
Example 5
The embodiment provides a tooth anti-sensitive toothpaste, which comprises the following components in percentage by weight:
10% of bagasse calcium phosphate composite material of example 1, 10% of silicon dioxide, 35% of glycerol, 15% of sorbitol, 0.4% of xanthan gum, 0.4% of carrageenan, 0.5% of sodium carboxymethyl cellulose, 1.5% of peppermint essence, 0.5% of sodium benzoate, 0.3% of saccharin sodium, 2% of sodium lauryl sulfate, 3% of potassium nitrate and the balance of water.
The preparation method of the tooth anti-sensitive toothpaste provided in the embodiment is basically the same as that in embodiment 4, wherein potassium nitrate is added in step 1).
Example 6
The embodiment provides toothpaste, which comprises the following components in percentage by weight:
5% of bagasse calcium phosphate composite material of example 2, 15% of silicon dioxide, 35% of glycerol, 15% of sorbitol, 5% of silicon dioxide, 0.5% of xanthan gum, 0.3% of carrageenan, 0.5% of sodium carboxymethyl cellulose, 1.5% of peppermint flavor, 0.5% of sodium benzoate, 0.3% of saccharin sodium, 2% of sodium lauryl sulfate and the balance of water.
The toothpaste provided in this example was prepared in the same manner as in example 4.
Comparative example 1
This comparative example provides a toothpaste that differs from example 4 only in that the bagasse calcium phosphate composite is replaced with an equivalent amount of abrasive monocalcium phosphate.
The toothpaste provided in this comparative example was prepared in the same manner as in example 4.
Comparative example 2
This comparative example provides a dental anti-sensitivity toothpaste that differs from example 5 only in that the bagasse calcium phosphate composite is replaced with an equivalent amount of abrasive monocalcium phosphate.
The preparation method of the tooth anti-sensitive toothpaste provided in the comparative example is the same as that in example 5.
Comparative example 3
This comparative example provides a toothpaste that differs from example 6 in that the bagasse calcium phosphate composite is replaced with an equivalent amount of abrasive monocalcium phosphate.
The toothpaste provided in this comparative example was prepared in the same manner as in example 6.
Test example 1
Whiteness detection
The whiteness of the toothpaste was tested using a WSD-III type automatic whiteness meter. The whiteness test results of the toothpastes of example 4 and comparative example 1 are shown in Table 1.
TABLE 1
Toothpaste sample Whiteness degree
Example 4 95
Comparative example 1 95
The results show that: the whiteness of the toothpastes of example 4 and comparative example 1 are substantially identical, demonstrating that the bagasse calcium phosphate composite of the present invention, as an abrasive for toothpastes, can achieve substantially the same paste appearance properties as the abrasive monocalcium phosphate.
Test example 2
Cleaning force test
1.0g of toothpaste sample is weighed and placed on a white organic glass plate attached with special dirt on a cleaning value tester, a nose with a soft bristle toothbrush is put down, so that the bristles are in close contact with the organic glass plate, the instrument is started, and the toothbrush moves back and forth immediately to rub the organic glass plate. After rubbing for 20 times, 50 times, 100 times, 150 times, 200 times and 300 times in sequence, the organic glass plate is taken out and put into a whiteness meter to measure corresponding data. The 6 data are converted into a cleaning value CV. Higher CV values indicate more cleaning power of the toothpaste. The results of the test of the cleaning values of the toothpastes of example 5 and comparative example 2 are shown in Table 2.
TABLE 2
Toothpaste sample CV value
Examples5 24
Comparative example 2 19.7
The results show that: when 10% of the abrasive monocalcium phosphate in the toothpaste is replaced by the bagasse calcium phosphate composite material of the embodiment of the invention, the cleaning value of the toothpaste is increased from 19.7 to 24, and the cleaning value is improved by more than 20%, which shows that compared with the abrasive monocalcium phosphate, the bagasse calcium phosphate composite material of the embodiment of the invention has excellent tooth cleaning performance as the abrasive for the toothpaste.
Test example 3
In vitro dentin tubule experiment
Cutting dentin sheet with thickness of about 3mm at 1-4mm position under enamel dentin boundary perpendicular to long axis direction of dentin with hard tissue cutter, sequentially grinding with sand paper on horizontal grinder, polishing to obtain dentin sheet with thickness of about 2mm, ultrasonic cleaning, etching with 6% citric acid for 2min, washing with distilled water for 30S, and blow drying to obtain sensitive dentin. The tooth brushing experiment was performed on sensitive dentin with the same toothbrush using the same concentration of the toothpaste slurry, and then SEM observation was performed on the surface and longitudinal section of the isolated dentin, and the occlusion rate (PR) of the isolated dentin tubule was calculated. The results of the tests for the clogging rate of the dental anti-sensitive toothpaste of example 5 and comparative example 2 are shown in Table 3.
TABLE 3 Table 3
Toothpaste sample PR value
Example 5 93%
Comparative example 2 20%
The results show that: when 10% of abrasive monocalcium phosphate in the tooth anti-sensitive toothpaste is used for replacing the bagasse calcium phosphate composite material in the embodiment of the invention, the in-vitro dentinal tubule blocking rate of the tooth anti-sensitive toothpaste is obviously increased, and the blocking rate reaches more than 90%, which indicates that compared with the abrasive monocalcium phosphate, the bagasse calcium phosphate composite material in the embodiment of the invention has more excellent desensitizing effect when being used as the abrasive and anti-sensitive component for the tooth anti-sensitive toothpaste.
Test example 4
Taste test brush
60 volunteers with healthy oral cavity were randomly selected and grouped into experiments 1-4, each group being 15. Among them, the volunteer of experiment 1 used the toothpaste of example 5, the volunteer of experiment 2 used the toothpaste of comparative example 2, the volunteer of experiment 3 used the toothpaste of example 6, and the volunteer of experiment 4 used the toothpaste of comparative example 3. All volunteers used the personal habit brushing regimen in a unified manner using a toothbrush provided by Yunnan white drug group Co., ltd. Filling out a questionnaire for the mouth feel of the toothpaste after 3 days, and obtaining a result through statistics. Wherein:
like: the taste is fine and smooth, and no granular feel exists;
generally: the taste is rough, and the friction feeling of particles is obvious;
dislike: has a rough taste and obvious granular friction feeling.
The test results are shown in Table 4.
TABLE 4 Table 4
Group of Toothpaste sample Xi Huan In general Dislike Preference degree
Experiment 1 group Example 5 12 2 1 80%
Experiment 2 group Comparative example 2 8 2 5 53.3%
Experiment 3 group Example 6 9 2 4 60%
Experiment 4 group Comparative example 3 8 3 4 53.3%
The results show that: when 5% of the abrasive monocalcium phosphate in the toothpaste was replaced with the bagasse calcium phosphate composite material of the present examples, the brushing mouthfeel of the toothpaste was substantially unchanged (see experiments 3-4); when 10% of the abrasive calcium dihydrogen phosphate in the toothpaste is used for replacing the bagasse calcium phosphate composite material of the embodiment of the invention, the taste preference of the toothpaste in a brushing test is increased by more than 20% (see experiment 1-2 groups), and the above description shows that compared with the abrasive calcium dihydrogen phosphate, the bagasse calcium phosphate composite material of the embodiment of the invention can be accepted and favored by the public when being added into the toothpaste.
While the invention has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.

Claims (5)

1. The preparation method of the bagasse calcium phosphate composite material is characterized in that bagasse is used as a raw material, and sequentially undergoes a phosphate reaction, a calcium hydroxide neutralization reaction, centrifugal separation, drying and grinding to obtain the bagasse calcium phosphate composite material; the concentration of phosphoric acid used in the phosphorylation reaction is 30% -80%, and the mass ratio of bagasse to phosphoric acid is 1 (3-8);
the temperature of the phosphorylation reaction is 70-200 ℃ and the time is 2-4 hours; the molar ratio of the calcium hydroxide to the phosphoric acid is (1-1.02): 1;
the temperature of the neutralization reaction of the calcium hydroxide is 70-80 ℃ and the time is 0.5-2 h; after the calcium hydroxide neutralization reaction is finished, regulating the pH value of the system to be 6.75-7.50; the grain diameter of the bagasse calcium phosphate composite material is 0.1-50 microns; the preparation method of the bagasse comprises the following steps: and (3) after the sugar is squeezed from the sugarcane, adding water for ball milling until the leaching solution is clear and transparent, sieving with a water sieve with more than 40 meshes, removing large particles, drying the undersize and carrying out jet milling to obtain powder with the particle size of 0.1-50 microns.
2. A bagasse calcium phosphate composite material, characterized in that it is produced by the preparation method of claim 1.
3. Use of the bagasse calcium phosphate composite material according to claim 2 as at least one of an abrasive, an anti-sensitization ingredient, in the manufacture of an oral care product.
4. The use according to claim 3, wherein the oral care product is a toothpaste, a dentifrice or a tooth desensitizing agent.
5. A toothpaste, characterized in that the toothpaste comprises the bagasse calcium phosphate composite material according to claim 2, wherein the bagasse calcium phosphate composite material accounts for 0.1% -70% of the toothpaste by mass;
the toothpaste also comprises at least one of humectant, binder, abrasive, essence, antiseptic, sweetener, foaming agent and water.
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Publication number Priority date Publication date Assignee Title
JPH1198971A (en) * 1997-09-26 1999-04-13 Nisshin Sugar Mfg Co Ltd Caries resisting agent and food and beverage containing the same
CN106074195A (en) * 2016-07-06 2016-11-09 杭州皎洁口腔保健用品有限公司 A kind of toothpaste of hydroxyl apatite and calcium carbonate and preparation method thereof
CN107929192A (en) * 2017-11-13 2018-04-20 常州凯恒纺织品有限公司 A kind of antiallergic sense toothpaste

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1198971A (en) * 1997-09-26 1999-04-13 Nisshin Sugar Mfg Co Ltd Caries resisting agent and food and beverage containing the same
CN106074195A (en) * 2016-07-06 2016-11-09 杭州皎洁口腔保健用品有限公司 A kind of toothpaste of hydroxyl apatite and calcium carbonate and preparation method thereof
CN107929192A (en) * 2017-11-13 2018-04-20 常州凯恒纺织品有限公司 A kind of antiallergic sense toothpaste

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