Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide the antibacterial spinning oil which has simple components, is convenient to operate, can be directly applied without subsequent compounding and is suitable for acetate fibers for cigarette filter sticks.
The invention provides an antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks, which comprises an emulsifier, a mineral agent, a fat-soluble antibacterial agent and water or water containing the water-soluble antibacterial agent, wherein the spinning oil is transparent water-in-oil liquid before phase inversion, is oil-in-water emulsion after phase inversion, is carried out in water or water containing the water-soluble antibacterial agent, and has the mass ratio of (1-49) to the water containing the water-soluble antibacterial agent before phase inversion: (99-51).
Preferably, in the antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks provided by the invention, the mass ratio of the spinning oil before phase inversion to the water for phase inversion or the water containing water-soluble antibacterial agent is (1-20): (99-80).
Preferably, in the antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks provided by the invention, the fat-soluble antibacterial agent is one or more of benzoic acid, sorbic acid, ethyl parahydroxybenzoate and propyl parahydroxybenzoate, and the mass ratio of the fat-soluble antibacterial agent to mineral oil before phase inversion is (0.1-100): (99.9-0).
Preferably, in the antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks, the ratio of the emulsifier before phase inversion in the spinning oil before phase inversion is 18-60 wt%, the total ratio of the fat-soluble antibacterial agent before phase inversion and the mineral oil before phase inversion in the spinning oil before phase inversion is 30-80 wt%, and the ratio of the water before phase inversion or the water containing the water-soluble antibacterial agent in the spinning oil before phase inversion is 3-20 wt%.
Still preferably, in the antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks provided by the invention, the ratio of the emulsifier before phase inversion in the spinning oil before phase inversion is 20-50 wt%, the ratio of the fat-soluble antibacterial agent before phase inversion and the mineral oil before phase inversion in the spinning oil before phase inversion is 40-80 wt%, and the ratio of the water before phase inversion or the water containing the water-soluble antibacterial agent in the spinning oil before phase inversion is 3-15 wt%.
Preferably, in the antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks, the emulsifier is a mixture of any one of food-grade span 20-50 and any one of food-grade tween 40-80.
Preferably, in the antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks, one or more of glyceryl monostearate, xylitol anhydride monostearate, polyoxyethylene xylitol anhydride monostearate and fatty acid sucrose ester are further contained in the emulsifier mixture.
Preferably, in the antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks provided by the invention, the mineral oil is food-grade white oil.
Preferably, in the antibacterial spinning oil suitable for acetate fibers for cigarette filter sticks provided by the invention, the water-soluble antibacterial agent is one or more of 4-chloro-3-cresol, dichlorophenoxychlorophenol, bromochlorobisphenol, benzalkonium chloride, dodecyldimethyl ethylbenzene oxyethyl ammonium bromide, guanidine and guanidine polymers, quaternary ammonium salt, silver ion, copper ion, sodium benzoate, nephelene, dimethyl fumarate and dehydroacetic acid; the mass ratio of the water solvent antibacterial agent to water in water containing the water-soluble antibacterial agent before phase inversion is (0.1-100): (99.9 to 0); the mass ratio of the water solvent antibacterial agent to water in the water containing the water-soluble antibacterial agent for phase inversion is (0.1-100): (99.9-0).
In addition, the invention also discloses a preparation method of the antibacterial spinning oil suitable for the acetate fiber for the cigarette filter stick, which comprises the following steps:
(1) Firstly, respectively dissolving a fat-soluble antibacterial agent in mineral oil and dissolving a water-soluble antibacterial agent in water according to the proportion to prepare antibacterial mineral oil containing the fat-soluble antibacterial agent and antibacterial water containing the water-soluble antibacterial agent; then the antibacterial oil, the emulsifier and the antibacterial water are prepared into spinning oil according to the proportion.
(2) Firstly, dissolving the fat-soluble antibacterial agent in mineral oil according to the proportion to prepare antibacterial mineral oil containing the fat-soluble antibacterial agent, and then mixing the antibacterial mineral oil, the water-soluble antibacterial agent, water and an emulsifying agent together to prepare the spinning oil.
(3) Firstly, dissolving the fat-soluble antibacterial agent in mineral oil according to the proportion to prepare antibacterial mineral oil containing the fat-soluble antibacterial agent, and then mixing the antibacterial mineral oil, water and an emulsifying agent together to prepare the spinning oil.
(4) Firstly, dissolving a water-soluble antibacterial agent in water according to the proportion to prepare antibacterial water containing the water-soluble antibacterial agent, and then mixing the fat-soluble antibacterial agent, mineral oil, the antibacterial water and an emulsifying agent together according to the proportion to prepare the spinning oil.
(5) The fat-soluble antibacterial agent, mineral oil, water and emulsifying agent are mixed together according to the proportion to prepare the spinning oil.
(6) The fat-soluble antibacterial agent, mineral oil, water-soluble antibacterial agent and emulsifying agent are mixed together according to the proportion to prepare the spinning oil.
(7) The spinning oil prepared in (1) or (2) or (3) or (4) or (5) or (6) is subjected to phase inversion in water or water containing an antibacterial agent.
The technical scheme of the invention has the advantages that: (1) The spinning method can be directly applied to the spinning of acetate fibers after phase inversion without subsequent compounding. (2) The antibacterial agent is a fat-soluble compound, the antibacterial agent is added into mineral oil to prepare antibacterial mineral oil, and then the antibacterial mineral oil, the emulsifying agent and water are used together to prepare spinning oil, so that the emulsification effect is good, and the antibacterial oil has few components. (3) The method has the advantages of few types of chemicals, simple operation and high safety performance, and is suitable for large-scale industrial continuous production. (4) The spinning oil after phase inversion is milky, odorless and nontoxic, has good antibacterial effect, is suitable for processing acetate fiber for cigarettes, and does not affect the flavor of cigarettes. (5) The spinning oil before phase inversion is not layered and precipitated, and can be stored for a long time.
Detailed Description
The invention provides an antibacterial spinning oil for acetate fibers for cigarette filter sticks, which comprises an emulsifier, an oil agent, a fat-soluble antibacterial agent and water or water containing the water-soluble antibacterial agent. The spinning oil before phase inversion is light yellow to colorless transparent water-in-oil liquid, and is subjected to phase inversion in water or water containing an antibacterial agent, and the phase inversion is an oil-in-water type white emulsion. The phase inversion can be directly applied to the spinning process.
With respect to the emulsifier. The emulsifier is a mixture of any one of food-grade span 20-50 and any one of food-grade tween 40-80, and can also contain other food emulsifiers, such as glyceryl monostearate, xylitol anhydride monostearate, polyoxyethylene xylitol anhydride monostearate and fatty acid sucrose ester.
Before phase inversion, the ratio of the emulsifier in the spinning oil is 18-60 wt%; if the ratio is less than 18wt%, a stable emulsion cannot be formed; if the weight percentage exceeds 60%, the viscosity and density of the spinning oil cannot meet the requirements, and the phase cannot be inverted in the subsequent operation; a further preferred proportion is 20% to 50% by weight.
With respect to mineral oils, food grade white oils are preferred. Commercially available mineral oils are clear liquids ranging from colorless to yellow or brown. Before phase inversion, the ratio of mineral oil in the spinning oil is 30-80 wt%; if it is less than 30wt%, a stable water-in-oil emulsion cannot be formed; if the ratio is higher than 80wt%, the phase cannot be inverted in the subsequent operation to form a usable spin finish; a further preferred proportion is 45 to 80% by weight.
With respect to liposoluble antibacterial agents. The antibacterial agent can be selected from commercial cosmetic bactericide or food antiseptic or medical and health bactericide, such as one or more of benzoic acid, sorbic acid, ethyl p-hydroxybenzoate, and propyl p-hydroxybenzoate.
The preparation of mineral oils containing antimicrobial agents has two methods: (1) Adding the fat-soluble antibacterial agent into mineral oil in advance to prepare mineral oil with the antibacterial agent concentration of 0.1-100 wt%, and then mixing the mineral oil with an emulsifying agent and water or water containing the water-soluble antibacterial agent to prepare spinning oil; (2) Directly mixing the fat-soluble antibacterial agent with mineral oil, an emulsifying agent and water or water containing the water-soluble antibacterial agent to prepare the spinning oil. Regardless of the preparation method, the ratio of the mineral oil containing the antibacterial agent before the phase inversion in the spinning oil before the phase inversion is 3-20 wt%, and more preferably 3-15 wt%.
Regarding the ratio of the spin finish before inversion to the inversion water or water containing the water-soluble antibacterial agent. The mass ratio of the two is (1-49): (99 to 51), preferably (1 to 30): (99-80).
The application method of the spinning oil comprises the following steps: the prepared light yellow to colorless transparent water-in-oil spinning oil is directly poured into water or water containing an antibacterial agent for phase inversion, and the spinning oil after phase inversion is oil-in-water type, is milky white and can be directly used by users.
Example 1
An antibacterial spinning oil for acetate fibre used for cigarette filter stick is prepared from emulsifier, antibacterial mineral oil and water through phase inversion in antibacterial water.
The emulsifier is a mixture of food grade span 50 and food grade tween 80.
Preparing antibacterial mineral oil: the liposoluble antibacterial agent is benzoic acid. Benzoic acid is also known as benzoic acid, and is in a solid state. The mineral oil is food grade white oil. Benzoic acid and food-grade white oil are mixed according to the mass ratio of 0.1:99.9.
The prepared antibacterial mineral oil, the selected emulsifier and water are put together to prepare spinning oil, wherein the water accounts for 20wt% of the spinning oil before the prepared phase inversion, the emulsifier accounts for 18wt% of the spinning oil before the prepared phase inversion, and the antibacterial mineral oil accounts for 62wt% of the spinning oil before the prepared phase inversion.
Preparation of antibacterial water for phase inversion: the commercial quaternary ammonium salt antibacterial agent is selected to be water-soluble liquid. The selected quaternary ammonium salt antibacterial agent liquid is added into water to prepare antibacterial water with the antibacterial agent content of 0.2 wt%.
The spinning oil before phase inversion and antibacterial water for phase inversion are mixed according to the mass ratio of 1:99 to perform phase inversion. The spinning oil before phase inversion is light yellow transparent liquid, no suspended matters or sediment exists, the spinning oil before phase inversion is water-in-oil type, and the spinning oil after phase inversion is oil-in-water type and is milky. No delamination occurred after 1 month of standing of the spin finish before and after the phase inversion.
Example 2
The emulsifier is a mixture of span 50, tween 80 and glyceryl monostearate.
Preparing antibacterial mineral oil: the liposoluble antibacterial agent is ethyl p-hydroxybenzoate. Commercial ethyl parahydroxybenzoate is colorless or white crystalline powder, almost odorless. The mineral oil is food grade white oil. The mass ratio of the ethyl p-hydroxybenzoate to the mineral oil is 50: 50.
Preparing antibacterial water: the water-soluble antibacterial agent is commercial guanidine antibacterial agent, and the guanidine antibacterial agent is dissolved in water to prepare antibacterial water with the antibacterial agent content of 50wt%.
The spinning oil is prepared by mixing the prepared antibacterial mineral oil, the selected emulsifier and the antibacterial water. Wherein the ratio of the antibacterial mineral oil in the spinning oil before phase inversion is 77wt%; the antibacterial water accounts for 3wt% of the spinning oil before phase inversion; the ratio of the emulsifier in the spinning oil before phase inversion is 20wt%.
The mass ratio of the spinning oil before phase inversion to the antibacterial water used for phase inversion is 5:95.
The spinning oil before phase inversion is light yellow transparent liquid, no suspended matters or sediment exists, the spinning oil before phase inversion is water-in-oil type, and the spinning oil after phase inversion is oil-in-water type and is milky. No delamination occurred after 1 month of standing of the spin finish before and after the phase inversion.
Example 3
An antibacterial spinning oil for acetate fiber used for cigarette filter stick comprises antibacterial mineral oil, emulsifier, water-soluble antibacterial agent and water. The emulsifier is a mixture of span 30 and tween 60.
Preparing antibacterial mineral oil: the mineral oil is food-grade white oil; the liposoluble antibacterial agent is sorbic acid, which is colorless powder. Sorbic acid and mineral oil are mixed according to the mass ratio of 30:70.
The water-soluble antibacterial agent is commercially available benzalkonium chloride antibacterial agent, and the mass ratio of the benzalkonium chloride antibacterial agent to water in the spinning oil before phase inversion is 60:40.
The spinning oil is prepared by mixing the prepared antibacterial mineral oil, the selected emulsifier, the selected zachlor-ammonium antibacterial agent and water. Wherein the total proportion of the water and the zachlor-ammonium antibacterial agent in the prepared spinning oil before phase inversion is 5wt%; the ratio of the emulsifier in the spinning oil before the prepared phase inversion is 60wt%; the antibacterial mineral oil accounts for 35wt% of the spinning oil before phase inversion. Water is adopted for phase inversion. The mass ratio of spinning oil before phase inversion to water for phase inversion is 20:80.
the antibacterial spinning oil before phase inversion is light yellow transparent liquid, no suspended matters or sediment exists, and the spinning oil before phase inversion is water-in-oil type; the spinning oil after phase inversion is oil-in-water type and is milky white. No delamination occurred after 1 month of standing of the spin finish before and after the phase inversion.
Example 4
The emulsifier is mixture of span 20, tween 40 and xylitol monostearate, and the mineral oil is food-grade white oil. The fat-soluble antibacterial agent is propyl p-hydroxybenzoate. Propyl parahydroxybenzoate is commercially available as a colorless or white powder.
The spinning oil is prepared by directly mixing propyl p-hydroxybenzoate, food-grade white oil, selected emulsifier and water without preparing antibacterial mineral oil in advance. Wherein the mass ratio of the propyl parahydroxybenzoate to the mineral oil before transfer phase is 60:40, a step of performing a; the water accounts for 5wt% of the spinning oil before the phase inversion, the emulsifier accounts for 45wt% of the spinning oil before the phase inversion, and the total of the propyl p-hydroxybenzoate and the food-grade white oil accounts for 45wt% of the spinning oil before the phase inversion.
The inversion uses water containing water-soluble antimicrobial agent: the water-soluble antibacterial agent is commercially available silver ion antibacterial agent. In the water containing the water-soluble antibacterial agent for phase inversion, the mass ratio of the antibacterial agent to the water is 0.1:99.9.
The prepared spinning oil is subjected to phase inversion in water containing a water-soluble antibacterial agent, and the mass ratio of the spinning oil before phase inversion to the water containing the water-soluble antibacterial agent for phase inversion is 30:70.
the antibacterial spinning oil before phase inversion is light yellow transparent liquid, no suspended matters or sediment exists, and the spinning oil before phase inversion is water-in-oil type; the spinning oil after phase inversion is oil-in-water type and is milky white. No delamination occurred after 1 month of standing of the spin finish before and after the phase inversion.
Example 5
The emulsifier is a mixture of food grade span 40, food grade tween 50 and food grade xylitol anhydride monostearate, and the mineral oil is food grade white oil. The fat-soluble antibacterial agent is selected from propyl parahydroxybenzoate, which is colorless or white powder. The water-soluble antibacterial agent is commercially available sodium benzoate antibacterial agent.
The spinning oil is prepared by directly mixing propyl p-hydroxybenzoate, food-grade white oil, selected emulsifier, sodium benzoate antibacterial agent and water without preparing antibacterial mineral oil in advance. Wherein the mass ratio of the propyl parahydroxybenzoate to the mineral oil before transfer phase is 45:55; the mass ratio of the sodium phenylpropionate antibacterial agent before phase inversion to the water before phase inversion is 5:95; the total proportion of sodium propionate antibacterial agent and water in the spinning oil before the prepared phase inversion is 15wt%; the total ratio of propyl parahydroxybenzoate to food-grade white oil in the spinning oil before phase inversion is 35wt%; the ratio of the emulsifier in the spinning oil before the phase inversion is 50wt%,
the phase inversion is carried out using water containing a water-soluble antimicrobial agent. The water-soluble antibacterial agent is commercially available silver ion antibacterial agent. In the water containing the water-soluble antibacterial agent for phase inversion, the mass ratio of the silver ion antibacterial agent to the water is 1:99. The mass ratio of spinning oil before phase inversion to water containing water-soluble antibacterial agent for phase inversion is 30:70.
the antibacterial spinning oil before phase inversion is light yellow transparent liquid, no suspended matters or sediment exists, and the spinning oil before phase inversion is water-in-oil type; the spinning oil after phase inversion is oil-in-water type and is milky white. No delamination occurred after 1 month of standing of the spin finish before and after the phase inversion.
Example 6
The water-soluble antibacterial agent is commercially available dimethyl fumarate antibacterial agent. The emulsifier is a mixture of span 30, tween 40 and sucrose fatty acid ester. The mineral oil is food grade white oil. The liposoluble antibacterial agent is sorbic acid and benzoic acid.
Preparation of antibacterial water in spinning oil before phase inversion: the commercial dimethyl fumarate antibacterial agent is dissolved in water to prepare antibacterial water, wherein the mass ratio of the antibacterial agent dimethyl fumarate to the water is 30:70.
Firstly, mixing 60wt% of emulsifying agent, 30wt% of food-grade white oil, sorbic acid and benzoic acid, and 10wt% of antibacterial water together to prepare spinning oil; and then the prepared spinning oil is subjected to phase inversion in antibacterial water to obtain the spinning oil which is directly used in the spinning process.
The concentration of the antibacterial water for phase inversion is 20wt%, and the antibacterial agent in the antibacterial water for phase inversion is a commercial dehydroacetic antibacterial agent; the mass percentage of spinning oil before phase inversion and antibacterial water for phase inversion is 40:60.
the spinning oil after phase inversion is oil-in-water type and is milky. After standing for 1 month, the spinning emulsion before and after phase inversion is not layered.
Example 7
The transparent spinning oil solutions prepared in examples 1 to 6 were tested according to QB/T2738-2012 evaluation method for antibacterial and bacteriostatic effects of daily chemical products, and the test results are shown in Table 1.
Table 1 results of measuring antibacterial properties of spin finishes prepared in examples 1 to 6
According to QB/T2738-2012, the method for evaluating the antibacterial and bacteriostatic effects of daily chemical products is as follows: the antibacterial rate is greater than or equal to 50% -90%, and the product has antibacterial effect; the antibacterial rate is more than or equal to 90%, and the product has a strong antibacterial effect.
It can be seen that the pale yellow spinning oil prepared in examples 1 to 6 has a strong antibacterial effect. In addition, the spinning oil provided by the invention is in a stable state no matter before or after phase inversion, does not delaminate, and has a viscosity of 60-70 mm measured at 37.8 DEG C 2 And the range of/s meets the requirement of convenient subsequent operation.