WO2020073677A1 - Discoloring friction particles for toothpaste and preparation method therefor - Google Patents

Abstract

The present invention belongs to the technical field of silica, and specifically relates to discoloring friction particles for a toothpaste and a preparation method therefor. The method of the present invention comprises: putting a colored silica into a pelletizer, setting the frequency of a fan, and the revolving speed of a liquid supply, etc., turning on the sealing of a vessel, turning on the fan, starting a program, manually raising a turntable, turning on the turntable, injecting and blowing, and ventilating, spraying a carboxymethyl cellulose solution; and spraying to form particles having a particle size of 120-150 mesh, splashing a starch therein, spraying a mixed solution of carboxymethyl cellulose and xanthan gum until particles having a particle size of 50-70 mesh are formed, turning on the heating, turning off the spraying, ventilating, injecting and blowing, heating and the turntable, manually lowering the turntable, and then turning off the program, the fan, and the sealing of the vessel, taking the materials out, and drying and sieving same, thereby making the discoloring friction particles for a toothpaste. The discoloring friction particles of the present invention can be used as a friction agent added into a toothpaste directly, achieving the dual effects of mouth cleaning and discoloration hints, and have good application prospects.

Description

Color-changing friction particles for toothpaste and preparation method thereof Technical field

The invention belongs to the technical field of silica, and particularly relates to a color-changing friction particle for toothpaste and a preparation method thereof.

Background technique

With the improvement of living standards, people pay more and more attention to oral health and cleanliness. Brushing your teeth is an important self-oral health care method that uses a toothbrush to remove plaque, soft dirt and food debris, and keep your mouth clean. It is also the most important way for people to remove plaque by themselves to prevent the occurrence, development and recurrence of periodontal disease. However, people have 28 to 32 teeth, and the toothbrush head can only cover the position of two teeth, so it takes a certain time to ensure that all the upper, lower, inner and outer are brushed in place, so the specialist recommends that you must brush your teeth for three minutes, at least It also takes two minutes, otherwise the toothbrush will be inadequate and will not be able to clean your teeth. However, when people brush their teeth, it is often difficult to accurately control the time of the toothbrush, so the color-changing oral cleaning supplies come into being.

For example, the patent document CN 104797297 A discloses a dentifrice composition that changes color when brushing teeth. The composition includes a film substrate, a polymer material, and a second pigment. The film substrate is bonded to the second pigment through the polymer material. The film substrate includes a water-soluble polymer matrix (including polyvinylpyrrolidone, hydroxypropylmethyl cellulose, starch, thickener, propylene glycol, emulsifier, etc.) that can release the first pigment after being dissolved. The second pigment is powder particles such as titanium dioxide. The composition is suspended in the dentifrice, and after brushing teeth in the oral cavity in the presence of water for a period of more than 30 seconds and less than 180 seconds, where the matrix is substantially dissolved, the first pigment is released, providing the user with adequate brushing Color change signal.

Another example is the patent document CN 106963662 A which discloses a color-changing toothpaste for children, in which a microcapsule containing pigment is added, the microcapsule containing pigment contains water, glycerin, sorbitol, pigment, carrageenan, agar and butylated Vinylpyrrolidone and other preparation materials, the capsule softens and ruptures under the force of brushing teeth and the abrasive of the paste, and the wrapped pigment gradually disperses, the color of the foam changes, and a sufficient color signal prompt for brushing is formed.

The above-mentioned oral cleaning products all achieve the purpose of prompting the brushing time to reach 2 to 3 minutes by adding a color-changing substance. However, adding such raw materials will increase the cost of toothpaste and make the preparation process of toothpaste complicated.

Silica colored friction particles are widely used in toothpaste formulations as friction agents because of their stable physical and chemical properties, bright colors, and high safety performance. However, with the rapid development of society, consumers have higher requirements for product innovation and novelty. If you can develop a kind of friction particles that will change color after 2 to 3 minutes of brushing your teeth, remind consumers to achieve effective brushing time and ensure consumers ’brushing effect. This will be very attractive to consumers and go further It has promoted the development of the toothpaste industry. However, there is still a lack of such products on the market, so it is very necessary to develop a color-changing friction particle for toothpaste.

Patent document CN 107569401 A discloses a method for preparing toothpaste-coated particles with silica. A cooling agent and abrasive silica are bonded to form a core through a hydroxypropyl methylcellulose solution, and then a layer of silica shell is coated. And control the particle size in each step, so as to obtain a packaged particle that can make the cooling agent stable and slow-release in toothpaste, bring effective cleaning, long-lasting fresh mouth effect when used. Unfortunately, the wrapped particles split into small particles after only a few seconds of friction, and the effect of discoloration after a period of time cannot be achieved.

Summary of the invention

The present invention aims to provide a color-changing friction particle for toothpaste and a preparation method thereof, wherein colored friction silica particles are bonded by a carboxymethyl cellulose solution to form a colored core, and then starch, carboxymethyl cellulose and The mixed solution of xanthan gum forms a wrapped outer shell, and the toothpaste is prepared with color-changing friction particles. The particles can not only rub the mouth, but also change color after 2 to 3 minutes of brushing, thus reminding the user to achieve effective brushing time.

The preparation method of the color-changing friction particles for toothpaste of the present invention specifically includes the following steps:

The first step is to prepare a carboxymethyl cellulose solution and a mixed solution of carboxymethyl cellulose and xanthan gum;

The second step is to put colored silica into the pelletizer, set the fan frequency to 40 to 45 Hz, the liquid supply speed to 40 to 50 rpm, the turntable speed to 600 to 800 rpm, the inlet air temperature to 60 to 75 ° C, and the outlet air temperature to 40 ~ 50 ℃, then open the container to seal, turn on the fan for 30 seconds, start the program, manually raise the turntable, then turn the turntable, turn on the spray, turn on the ventilation for 2min, spray with carboxymethyl cellulose solution;

In the third step, after spraying to form spherical particles with a particle size of 120-150 mesh, sprinkle starch and spray with a mixture of carboxymethyl cellulose and xanthan gum until spherical particles with a particle size of 50-70 mesh are formed. Turn on the heating for 2min, turn off the spray, ventilate, spray, heat, turntable in turn, manually lower the turntable, then turn off the program, fan, container seal in turn, take out the materials, dry, sieve, and prepare the toothpaste with discolored friction particles.

Further, in the carboxymethyl cellulose solution, the mass percentage concentration of carboxymethyl cellulose is 2.0-4.0%.

Further, in the mixed solution of carboxymethyl cellulose and xanthan gum, the mass percentage concentration of carboxymethyl cellulose is 2.0-4.0%, and the mass percentage concentration of xanthan gum is 5.0-8.0%.

Furthermore, the colored silica is a friction type silica with a particle size of 500-800 mesh. The sensory, physical and chemical indexes of the frictional silica meet the requirements of QB / T2346-2007 "Silica for toothpaste".

Further, the colored silica includes blue silica, green silica and yellow silica.

Further, the added amount of the starch is 2 to 3.5 times that of colored silica.

In order to achieve the object of the present invention, it is first necessary to prepare a color core with a certain friction performance, and then select a shell material with suitable hardness, which is relatively easy to dissolve during the brushing process, and makes the color core develop color. Therefore, the preparation method of the color-changing friction particles for toothpaste of the present invention first uses a carboxymethyl cellulose solution as a binder, and binds the color friction type silica particles to each other until a particle size of 120 is obtained ~ 150 mesh spherical particles to obtain a colored core with a certain friction performance, and then sprayed into the mixed liquid of carboxymethyl cellulose and xanthan gum, at the same time sprinkle starch, starch combined with carboxymethyl cellulose and xanthan gum and colored core Wrap until spherical particles with a particle size of 50-70 mesh are obtained, and a white shell with suitable hardness and dissolution time is obtained. In the process of shell formation, the starch is mixed with carboxymethyl cellulose and xanthan gum to absorb and wrap, which can provide moderate viscosity and skeleton support for the shell, and ensure that the hardness of the shell is moderate.

The inventor found that by controlling the amount of materials fed, especially the amount of starch, carboxymethyl cellulose, xanthan gum when forming the shell, and the particle size of the material, the obtained discolored friction particles can be used as friction after being applied to toothpaste Agent, which provides the ability to clean the teeth by friction. On the other hand, during the brushing process, the outer shell of the discolored friction particles is wetted by water, and gradually becomes loose under the synergy of saliva amylase. After 2 to 3 minutes of brushing, the outer shell is completely dissolved, making The colored core is exposed, and the colored core immediately splits out colored silica to further clean the tooth gap, and also reminds the user that the effective brushing time has been reached.

Therefore, the color-changing friction particles for toothpaste obtained by the preparation method of the present invention can be directly added to the toothpaste as a friction agent, which achieves the dual effects of cleaning the oral cavity and discoloration prompt, and has good application prospects.

Therefore, compared with the prior art, the advantages of the present invention are:

The preparation method of the color-changing friction particles for toothpaste of the present invention is simple, the process is stable, the conditions are controllable, and it can be industrially produced. The prepared color-changing friction particles have both friction cleaning performance and color change prompting performance. Discoloration occurs after 3 minutes, which reminds the user to achieve effective brushing time, and has a good application prospect.

detailed description

The present invention will be described in detail below with reference to specific embodiments. Here, the exemplary embodiments and descriptions of the present invention are used to explain the present invention, but are not intended to limit the present invention.

The pill-making machine of the present invention is produced by Chongqing Jinggong Pharmaceutical Machinery Co., Ltd. and its model is FXL-60.

The blue friction type silica, green friction type silica, yellow friction type silica and white friction type silica of the present invention are all purchased from Guangzhou Feixue Chemical Co., Ltd. and the models are FX-B6 and FX respectively -G6, FX-Y6, FX-W1.

Example 1. Discolored friction particles for toothpaste of the present invention and preparation thereof

The first step is to prepare a carboxymethyl cellulose solution with a mass percentage concentration of 2.0%, and a mixed solution of carboxymethyl cellulose and xanthan gum; in the mixed solution of carboxymethyl cellulose and xanthan gum, carboxymethyl The mass percentage concentration of cellulose is 2.0%, and the mass percentage concentration of xanthan gum is 5.0%;

The second step is to put 10kg of blue abrasive silica with a particle size of 800 mesh into the pelletizer, and set the process conditions in the system program of the main electric control panel: fan frequency is 40Hz, liquid supply speed is 40rpm, turntable speed 600rpm, inlet air temperature is 60 ℃, outlet air temperature is 40 ℃; then open the container to seal, turn on the fan for 30 seconds, open the program (ie press the program start key to start the set system program), manually raise Turn the turntable, then turn the turntable, turn on the spray, turn on the ventilation for 2min, and spray with the carboxymethyl cellulose solution;

The third step is to spray to form regular and spherical particles with a particle size of 150 mesh, sprinkle 20kg of starch, and spray with a mixture of carboxymethyl cellulose and xanthan gum until spherical particles with a particle diameter of 70 mesh are formed and open After heating for 2min, turn off spray, aeration, blowing, heating, turntable in turn, manually lower turntable, then turn off the program, fan, container seal in turn, take out the materials, dry, sieve, and prepare the toothpaste with discolored friction particles.

Example 2. Discolored friction particles for toothpaste of the present invention and preparation thereof

The first step is to prepare a carboxymethyl cellulose solution with a mass percentage concentration of 4.0%, and a mixed solution of carboxymethyl cellulose and xanthan gum; in the mixed solution of carboxymethyl cellulose and xanthan gum, carboxymethyl The mass percentage concentration of cellulose is 4.0%, and the mass percentage concentration of xanthan gum is 8.0%;

The second step is to put 10kg of yellow abrasive silica with a particle size of 500 mesh into the pelletizer, and set the process conditions in the system program of the main electrical control cabinet panel: the fan frequency is 45Hz, the liquid supply speed is 50rpm, and the turntable speed is 800rpm, inlet air temperature is 75 ℃, outlet air temperature is 50 ℃; then open the container to seal, turn on the fan for 30 seconds, open the program (ie press the program start button to start the set system program), manually raise the turntable , Then turn on the turntable, turn on the spray, turn on the ventilation for 2min, and spray with the carboxymethyl cellulose solution;

The third step is to spray to form regular and spherical particles with a particle size of 120 mesh, sprinkle 35kg of starch, and spray with a mixture of carboxymethyl cellulose and xanthan gum until spherical particles with a particle size of 50 mesh are formed and open After heating for 2min, turn off spray, aeration, blowing, heating, turntable in turn, manually lower turntable, then turn off the program, fan, container seal in turn, take out the materials, dry, sieve, and prepare the toothpaste with discolored friction particles.

Example 3. Discolored friction particles for toothpaste of the present invention and preparation thereof

The first step is to prepare a carboxymethyl cellulose solution with a mass percentage concentration of 3.0%, and a mixed solution of carboxymethyl cellulose and xanthan gum; in the mixed solution of carboxymethyl cellulose and xanthan gum, carboxymethyl The mass percentage concentration of cellulose is 3.0%, and the mass percentage concentration of xanthan gum is 7.0%;

The second step is to put 10kg of green abrasive silica with a particle size of 600 mesh into the pelletizer, and set the process conditions in the system program of the main electric control panel: the fan frequency is 40Hz, the liquid supply speed is 45rpm, and the turntable speed is 700rpm, inlet air temperature is 70 ℃, outlet air temperature is 40 ℃; then open the container to seal, turn on the fan for 30 seconds, open the program (ie press the program start key to start the set system program), manually raise the turntable , Then turn on the turntable, turn on the spray, turn on the ventilation for 2min, and spray with the carboxymethyl cellulose solution;

The third step is to spray to form regular and spherical particles with a particle size of 140 mesh, sprinkle 25kg of starch, and spray with a mixture of carboxymethyl cellulose and xanthan gum until spherical particles with a particle size of 60 mesh are formed and open After heating for 2min, turn off spray, aeration, blowing, heating, turntable in turn, manually lower turntable, then turn off the program, fan, container seal in turn, take out the materials, dry, sieve, and prepare the toothpaste with discolored friction particles.

Example 4. Discolored friction particles for toothpaste of the present invention and preparation thereof

The first step is to prepare a carboxymethyl cellulose solution with a mass percentage concentration of 4.0%, and a mixed solution of carboxymethyl cellulose and xanthan gum; in the mixed solution of carboxymethyl cellulose and xanthan gum, carboxymethyl The mass percentage concentration of cellulose is 2.0%, and the mass percentage concentration of xanthan gum is 8.0%;

The second step is to put 10kg of green abrasive silica with a particle size of 800 mesh into the pelletizer, and set the process conditions in the system program of the main electric control panel: the fan frequency is 40Hz, the liquid supply speed is 40rpm, and the turntable speed is 600rpm, inlet air temperature is 75 ℃, outlet air temperature is 50 ℃; then open the container to seal, turn on the fan for 30 seconds, open the program (ie press the program start key to start the set system program), manually raise the turntable , Then turn on the turntable, turn on the spray, turn on the ventilation for 2min, and spray with the carboxymethyl cellulose solution;

The third step is to spray to form spherical particles with a regular size and a particle size of 120 mesh. Sprinkle 30kg of starch and spray with a mixture of carboxymethyl cellulose and xanthan gum until spherical particles with a particle size of 70 mesh are formed. After heating for 2min, turn off spray, aeration, blowing, heating, turntable in turn, manually lower turntable, then turn off the program, fan, container seal in turn, take out the material, dry, sieve, and make the toothpaste discoloration friction particles

Comparative example one

Compared with Example 3, this comparative example differs only in that: in the mixed solution of carboxymethyl cellulose and xanthan gum, the mass percentage concentration of carboxymethyl cellulose is 1.0%, and the mass percentage concentration of xanthan gum 9.0%;

Comparative Example 2

Compared with Example 3, this comparative example differs only in that: in the mixed solution of carboxymethyl cellulose and xanthan gum, the mass percentage concentration of carboxymethyl cellulose is 6.0%, and the mass percentage concentration of xanthan gum 4.0%;

Comparative example three

Compared with Example 3, this comparative example differs only in that the amount of starch added is 40 kg.

Comparative Example 4

Compared with Example 3, this comparative example differs only in that the amount of starch added is 15 kg.

Comparative Example 5

Compared with Example 3, this comparative example differs only in that: in the third step, after spraying to form regular and spherical particles with a particle size of 100 mesh, sprinkle 25 kg of starch.

Comparative Example 6

Compared with Example 3, this comparative example differs only in that: in the third step, after spraying to form regular and spherical particles with a particle size of 200 mesh, 25 kg of starch is sprinkled.

Comparative Example 7

Compared with Example 3, this comparative example differs only in that: in the third step, sprinkle 25 kg of starch and spray with a mixture of carboxymethyl cellulose and xanthan gum until spherical particles with a particle size of 100 mesh are formed .

Comparative Example 8

Compared with Example 3, this comparative example differs only in that: in the third step, sprinkle 25 kg of starch and spray with a mixture of carboxymethyl cellulose and xanthan gum until spherical particles with a particle size of 40 mesh are formed .

Test Example 1. Application effect of the color-changing friction particles for toothpaste of the present invention

The color-changing friction particles of Examples 1 to 4 and Comparative Examples 1 to 8 were applied to toothpaste to prepare a white toothpaste. The toothpaste formula (content percentage) is as follows: sorbitol 45%, sodium carboxymethyl cellulose 1.0%, sodium saccharin 0.2%, polyethylene glycol 4%, sodium lauryl sulfate 2.2%, fragrance 1.0%, discoloration friction particles 7%, thickened silica 8%, white friction silica 4%, the balance is deionized water.

(1) Invite 40 volunteers to participate in the test, 20 men and 20 women, aged 20 to 28 years, randomly divided into 4 groups, 5 men and 5 women in each group, group A, group B, group C and D group. Volunteers in group A tried the toothpaste made from color-changing friction particles of Examples 1 to 3. Volunteers in group B tried the toothpaste made from color-changing friction particles in Example 4 and comparative examples 1-2, and volunteers in group C tried comparative examples 3-5. Toothpaste made of color-changing friction particles, volunteers in group D tried the toothpaste made of color-changing friction particles of comparative examples 6-8, and recorded the time for each group of volunteers to brush their teeth with the corresponding toothpaste. 1 shown.

(2) The RDA and PCR values of the above toothpaste were tested, and the results are shown in Table 1 below.

Table 1

Color changing friction particles	Discoloration time	RDA value	PCR value	PCR / RDA ratio
Example 1	2 ～ 3min	132	116	0.88
Example 2	2 ～ 3min	112	103	0.92
Example 3	2 ～ 3min	120	115	0.96
Example 4	2 ～ 3min	113	103	0.91
Comparative example one	3 ～ 5min	107	90	0.84
Comparative Example 2	1 ～ 3min	142	116	0.82
Comparative example three	3 ～ 5min	93	72	0.77
Comparative Example 4	1 ～ 3min	146	110	0.75
Comparative Example 5	1 ～ 2min	138	112	0.81
Comparative Example 6	2 ～ 4min	111	93	0.84
Comparative Example 7	1 ～ 2min	95	70	0.74
Comparative Example 8	3 ～ 5min	114	98	0.86

It can be seen from Table 1 above:

(1) The toothpaste made of the color-changing friction particles of Examples 1 to 4 of the present invention will change color after brushing for 2 to 3 minutes, which will remind the user to achieve effective brushing time; The finished toothpaste has good friction and cleaning performance, the RDA value and PCR value are suitable, and the PCR / RDA ratio is high. Among them, the toothpaste made of the color-changing friction particles of Example 3 has the best friction and cleaning performance, so Example 3 is the present invention The best embodiment.

(2) Compared with Example 3, Comparative Example 1 and Comparative Example 2 changed the concentration of carboxymethyl cellulose and xanthan gum in the mixed solution. As a result, the discoloration time of the toothpaste of Comparative Example 1 was prolonged, and the friction and cleaning performance decreased. The discoloration time of the toothpaste of Comparative Example 2 is reduced, the RDA value (relative dentin loss value) is increased, and the PCR / RDA ratio is decreased. Long-term use will damage the enamel.

(3) Compared with Example 3, Comparative Example 3 and Comparative Example 4 increase and decrease the amount of starch respectively. As a result, the color change time of Comparative Example 3 toothpaste is prolonged, the friction and cleaning performance decreases, while the color change time of Comparative Example 4 toothpaste decreases. Short, RDA value increased significantly, PCR / RDA ratio decreased, long-term use will damage tooth enamel.

(4) Compared with Example 3, Comparative Examples 5 to 8 changed the particle size during the preparation process. As a result, the discoloration time of the toothpaste of Comparative Examples 5 and 7 was shortened, and the color of the Comparative Example 6 and Comparative Example 8 toothpastes The time is extended; in addition, the PCR / RDA ratios of the toothpastes in the comparative examples 5-8 are all decreased, suggesting that the friction and cleaning performance is reduced.

The above are only the preferred embodiments of the present invention. It should be noted that the above preferred embodiments should not be regarded as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. For those of ordinary skill in the art, without departing from the spirit and scope of the present invention, a number of improvements and retouches can also be made, and these improvements and retouches should also be considered as the scope of protection of the present invention.

Claims (7)

1. A preparation method of color-changing friction particles for toothpaste, characterized in that it includes the following steps:

   The first step is to prepare a carboxymethyl cellulose solution and a mixed solution of carboxymethyl cellulose and xanthan gum;

   The second step is to put colored silica into the pelletizer, set the fan frequency to 40 to 45 Hz, the liquid supply speed to 40 to 50 rpm, the turntable speed to 600 to 800 rpm, the inlet air temperature to 60 to 75 ° C, and the outlet air temperature to 40 ~ 50 ℃, then open the container to seal, turn on the fan for 30 seconds, start the program, manually raise the turntable, then turn the turntable, turn on the spray, turn on the ventilation for 2min, spray with carboxymethyl cellulose solution;

   In the third step, after spraying to form spherical particles with a particle size of 120-150 mesh, sprinkle starch and spray with a mixture of carboxymethyl cellulose and xanthan gum until spherical particles with a particle size of 50-70 mesh are formed. Turn on the heating for 2min, turn off the spray, ventilate, spray, heat, turntable in turn, manually lower the turntable, then turn off the program, fan, container seal in turn, take out the materials, dry, sieve, and prepare the toothpaste with discolored friction particles.
2. The method for preparing discolored friction particles for toothpaste according to claim 1, characterized in that, in the carboxymethyl cellulose solution, the mass percentage concentration of carboxymethyl cellulose is 2.0-4.0%.
3. The method for preparing discolored friction particles for toothpaste according to claim 1, characterized in that, in the mixed solution of carboxymethyl cellulose and xanthan gum, the mass percentage concentration of carboxymethyl cellulose is 2.0-4.0%, yellow The mass percentage concentration of the original gum is 5.0-8.0%.
4. The method for preparing color-changing friction particles for toothpaste according to claim 1, wherein the colored silica is a friction type silica with a particle size of 500-800 mesh.
5. The method for preparing discolored friction particles for toothpaste according to claim 1, wherein the colored silica includes blue silica, green silica, and yellow silica.
6. The method for preparing color-changing friction particles for toothpaste according to claim 1, characterized in that the addition amount of the starch is 2 to 3.5 times that of colored silica.
7. The color-changing friction particles for toothpaste prepared according to the method for preparing color-changing friction particles for toothpaste according to any one of claims 1 to 6.