CN111436557A - Magnetic deoxidizing preservative and preparation method thereof - Google Patents

Abstract

The invention belongs to the technical field of deoxygenation preservatives, and discloses a magnetic deoxygenation preservative and a preparation method thereof. The preparation method includes: activating iron powder, heating and activating iron powder with acid to obtain activated iron powder; preparing composite magnetic particles, dissolving ferric chloride and ferrous chloride in water, adding ammonia water under nitrogen protection to form a precipitate, and adjusting pH at the same time value, heating and reacting, separating the solid phase to obtain composite magnetic particles; the liquid ingredients are 1-3 parts by weight of the magnetic particles, 1-3 parts by weight oyster shell powder, 0.5-1.5 parts by weight vitamin C, 0.5-1. 1.0 parts by weight of tea polyphenols, 2-4 parts by weight of gum arabic, 1-3 parts by weight of modified starch, 2-4 parts by weight of sodium chloride and 0.5-1.5 parts by weight of ethanol, plus 50-60 parts by weight water to prepare a water mixture to obtain liquid ingredients; for papermaking, add the liquid ingredients to the pulp and send it to a paper machine for papermaking; compound and spray the activated iron powder on the surface of the paper to prepare a deoxidizing preservative. The magnetic deoxygenation preservative can effectively inhibit the growth of microorganisms.

Description

A kind of magnetic deoxidizing preservative and preparation method thereof

technical field

The invention relates to the technical field of deoxygenation preservatives, in particular to a magnetic deoxygenation preservative and a preparation method thereof.

Background technique

Deoxidizer is a chemical preservative widely recognized, accepted and applied in the food industry. It is made of non-toxic and harmless common chemical raw materials, does not contact with food, does not pollute food, has simple production process, low cost and good preservation effect. Deoxidizers are used to reduce the oxygen in the food environment to inhibit the growth and reproduction of aerobic microorganisms and insects, and prevent the oxidative deterioration of oils and fats. Corruption in the sales process.

At present, most of the deoxidizers produced in China are oxygen-absorbing and powdered. First, the effect of inhibiting the growth and reproduction of microorganisms is limited. Second, once leaked in the food packaging, it will contaminate the food and cause certain potential harm to the human body, which is not in line with green food. development requirements. Therefore, the present invention provides a magnetic deoxidizing fresh-keeping agent and a preparation method thereof, so as to solve the technical problems that the existing deoxidizing agent has limited effect on inhibiting the growth and reproduction of microorganisms and the deoxidizing agent is easy to leak.

SUMMARY OF THE INVENTION

In order to solve the technical problems in the prior art that the deoxidizer has limited effect of inhibiting the growth and reproduction of microorganisms and the deoxidizer is easy to leak, the present invention provides a magnetic deoxidizer and a preparation method thereof.

In order to solve the above-mentioned technical problems, the present invention adopts the following technical solutions:

A preparation method of a magnetic deoxygenation preservative, comprising the following steps:

Iron powder activation: The iron powder is heated and activated with acid to obtain activated iron powder;

Preparation of composite magnetic particles: Dissolving ferric chloride and ferrous chloride in water, adding ammonia water under nitrogen protection to form precipitation, adjusting pH value at the same time, heating the reaction, separating the solid phase, and obtaining composite magnetic particles;

The liquid ingredient is composed of 1-3 parts by weight of the magnetic particles, 1-3 parts by weight of oyster shell powder, 0.5-1.5 parts by weight of vitamin C, 0.5-1.0 parts by weight of tea polyphenols, 2-4 parts by weight of arabic glue, 1 to 3 parts by weight of modified starch, 2 to 4 parts by weight of sodium chloride and 0.5 to 1.5 parts by weight of ethanol, and 50 to 60 parts by weight of water to prepare a water mixture to obtain liquid ingredients;

In papermaking, the liquid ingredients are added to the pulp and sent to the paper machine to make paper;

Compounding and spraying the activated iron powder on the surface of the paper to prepare a deoxidizing preservative.

Preferably, the acid is hydrochloric acid or phosphoric acid. More preferably, in the iron powder activation process, add hydrochloric acid with a mass concentration of 5% to 25%, and add iron powder with a mass concentration of 10% to 20%; the temperature of the iron powder activation is 100 to 150 ° C, and the activation time is 30 to 60 minutes.

Preferably, in the preparation process of the composite magnetic particles, the mass ratio of ferric chloride and ferrous chloride is 1:2-2:1, and the total iron ion concentration is 0.1-0.3 mol/L.

Preferably, the pH value is maintained at 10 ± 0.1 by stirring, and the reaction is heated at 60 to 80 °C for 30 to 60 min, the solid phase is separated, washed with water until neutral, and then washed with absolute ethanol, and dried in vacuum at 70 °C.

Preferably, the mass of the liquid furnish accounts for 20-40% of the pulp.

Preferably, the liquid ingredients are added to the pulp, sent to a paper machine to filter water, press and dehydrate, and dry in a drying cylinder; spray the activated iron powder on the surface of the paper, dry, calender, and cut to obtain a finished product for deoxidation and preservation agent.

The deoxygenation preservative can be packaged in air-permeable wrapping paper, and the net contents of each small package are 1 g and 2 g respectively. The deoxidizer can also be directly cut into pieces and used in a food packaging bag, which can prevent children from accidentally eating the deoxidizer in the bag and improve safety.

Another object of the present invention is to provide a deoxygenation preservative prepared by the above preparation method, which can be used for deoxygenation insurance of various foods.

In the preparation method of the deoxidizing preservative provided by the present invention, the shell powder can absorb oxygen in the air, and form high-density oxygen around the iron powder and ferrous chloride, and the reduced iron powder and ferrous chloride are used as reducing agents , reacts with the oxygen in the air in the package, accelerates the oxidation reaction speed, deoxidizes rapidly, and can rapidly reduce the oxygen concentration. The amount of deoxygenation is increased; the growth of aerobic microorganisms is effectively inhibited. At the same time, gum arabic and modified starch enhance the strength of paper, absorb water, and provide a medium for oxidation reaction. Further, vitamin C and tea polyphenols are commonly used natural antioxidants to achieve synergistic antioxidant effects. The addition of ethanol can enhance the anti-mildew and fresh-keeping effect of the deoxidizer, and the shell powder also has an anti-bacterial effect. After the shelf life experiment, the food has no mildew. Secondly, because of the application of the magnetic material, the deoxidizing and preservative provided by the present invention is not easy to fall off, and the problem of easy leakage will not occur. The test results show that the deoxidizing preservative provided by the invention can make the oxygen concentration of the food packaging bag reach below 0.001%, and the oxygen absorption amount of the deoxidizing agent can reach 15.0-17 mL/g, effectively inhibiting the growth of aerobic microorganisms.

Detailed ways

The invention discloses a magnetic deoxidizing preservative and a preparation method thereof, and those skilled in the art can learn from the content of this paper and appropriately improve the process parameters to achieve. It should be particularly pointed out that all similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. The method and application of the present invention have been described through the preferred embodiments, and it is obvious that relevant persons can make changes or appropriate changes and combinations of the methods and applications described herein without departing from the content, spirit and scope of the present invention to achieve and Apply the technology of the present invention.

In order to enable those skilled in the art to better understand the present invention, the present invention will be further described in detail below with reference to specific embodiments.

Example 1

Iron powder was activated by adding hydrochloric acid with a mass concentration of 5%, adding iron powder with a mass concentration of 10%, and treating at 100° C. for 30 minutes.

For the preparation of composite magnetic particles, ferric chloride and ferrous chloride with a mass ratio of 1:2 were dissolved in water, so that the total iron ion concentration was 0.1 mol/L, and ammonia water was added under nitrogen protection to form a precipitate, and at the same time, vigorously stirred to maintain The pH value is about 10. After reacting at 60 °C for 30 min, the solid phase is separated, washed with water until neutral, and then washed with absolute ethanol, and vacuum dried at 70 °C to obtain composite magnetic particles.

Preparation of liquid ingredients: The following components in parts by weight, 1 part of composite magnetic particles, 1 part of oyster shell powder, 0.5 part of vitamin C, 0.5 part of tea polyphenols, 2 parts of gum arabic, 1 part of modified starch, 2 parts of sodium chloride , 0.5 part of ethanol and 50 parts of water to prepare a water mixture.

In papermaking, liquid ingredients are added to the pulp, and the quality of the liquid ingredients accounts for 20% of the pulp, which is sent to the paper machine to filter water, press dewatering, and dry in the dryer.

Compounding: Spray the activated iron powder on the surface of the paper, continue to dry, calender and roll into paper; according to the specification requirements, cut the deoxidized paper to obtain a deoxidized preservative, which is packaged with a breathable packaging film, and the net content of each small package is respectively 1g and 2g.

Example 2

Iron powder was activated by adding hydrochloric acid with a mass concentration of 25%, adding iron powder with a mass concentration of 20%, and treating at 150° C. for 60 minutes.

For the preparation of composite magnetic particles, ferric chloride and ferrous chloride with a mass ratio of 2:1 were dissolved in water, so that the total iron ion concentration was 0.3 mol/L, and ammonia water was added under nitrogen protection to form a precipitate. The pH value is about 10. After reacting at 80 °C for 60 min, the solid phase is separated, washed with water until neutral, and then washed with absolute ethanol, and vacuum dried at 70 °C to obtain composite magnetic particles.

The preparation of liquid ingredients is the following components by weight, 3 parts of composite magnetic particles, 3 parts of oyster shell powder, 1.5 parts of vitamin C, 1.0 parts of tea polyphenols, 4 parts of gum arabic, 3 parts of modified starch, 4 parts of sodium chloride , 1.5 parts of ethanol and 60 parts of water to prepare a water mixture.

In papermaking, liquid ingredients are added to the pulp, and the quality of the liquid ingredients accounts for 40% of the pulp, which is sent to the paper machine to filter water, press dewatering, and dry in the dryer.

Compounding: Spray the activated iron powder on the surface of the paper, continue to dry, calender and roll it into paper; cut the deoxidized paper according to the specifications to obtain the deoxidized preservative; pack it with a breathable packaging film, and the net content of each small package is respectively 1g and 2g.

Example 3

Iron powder was activated by adding hydrochloric acid with a mass concentration of 15%, adding iron powder with a mass concentration of 15%, and treating at 120° C. for 45 minutes.

Preparation of composite magnetic particles: Dissolve ferric chloride and ferrous chloride with a mass ratio of 1:1 in water to make the total iron ion concentration 0.2 mol/L, add ammonia water under nitrogen protection to form a precipitate, and stir vigorously at the same time to maintain pH The value is about 10. After reacting at 70°C for 45 minutes, the solid phase is separated, washed with water until neutral, then washed with absolute ethanol, and dried in vacuum at 70°C to obtain composite magnetic particles.

The preparation of liquid ingredients is the following components by weight, 2 parts of composite magnetic particles, 2 parts of oyster shell powder, 1 part of vitamin C, 0.8 parts of tea polyphenols, 3 parts of gum arabic, 2 parts of modified starch, 3 parts of sodium chloride, ethanol 1 part and 55 parts of water to make a water mixture.

In papermaking, liquid ingredients are added to the pulp, and the quality of the liquid ingredients accounts for 30% of the pulp, which is sent to the paper machine to filter water, press dewatering, and dry in the dryer.

Compounding: Spray the activated iron powder on the surface of the paper, continue to dry, calender and roll it into paper; cut the deoxidized paper according to the specifications to obtain the deoxidized preservative; pack it with a breathable packaging film, and the net content of each small package is respectively 1g and 2g.

Example 4

Commonly used deoxidizer: The same amount of iron powder and other required auxiliary materials as in the embodiment are made into an iron-based deoxidizer, and placed in a bag to make a bag-shaped deoxidizer.

4.1 Test of oxygen intake

A certain amount of the deoxidizer prepared in Example 3 and the commonly used deoxidizer are placed in a sealed container respectively, and the deoxidizer will consume the oxygen in the container, so that the concentration of oxygen in the container changes, and the method of gas chromatography or oxygen concentration is used to measure. The instrument measures the concentration of oxygen in the container at different times.

Oxygen uptake (ml/g)=(V1-V2)×500ml/W

Among them, V1 is the oxygen content in the blank bottle, %; V2 is the oxygen content in the sample bottle, %; 500ml is the volume of the measuring bottle; W is the sample mass g.

It is finally measured that the oxygen absorption capacity of the deoxidizer prepared in Example 3 of the present invention reaches 15.0-17.0 mL/g, which is better than 10.0-12.0 mL/g of the commonly used deoxidizer.

4.2 Deoxidation speed test

The deoxidizer prepared in Example 3 of the present invention can reduce the oxygen concentration of 1L25% in the food packaging bag to 1% within 24 hours (measured by gas chromatography), and the residual oxygen concentration in the final food packaging bag is below 0.001%.

4.3 Antioxidative rancidity and safety

The deoxygenation preservatives provided in Examples 1-3 have no spoilage, no discoloration, and the acid value is below the national standard. After the shelf life test, the food has no mildew. The LD ₅₀ of the deoxidizing preservative is >10g/kg, it is safe and non-toxic, and it is a whole. It is magnetic and will not drop iron powder, the ingredients will not leak, and it will not contaminate food.

The above tests show that the deoxygenation preservative prepared by the present invention does not leak and fall off, is pollution-free, is relatively safe, has a strong effect of inhibiting the growth and reproduction of microorganisms, and has a wide range of applications.

The above are only the preferred embodiments of the present invention. It should be pointed out that for those skilled in the art, without departing from the principles of the present invention, several improvements and modifications can be made. It should be regarded as the protection scope of the present invention.

Claims (9)

1. A preparation method of a magnetic deoxidizing preservative is characterized by comprising the following steps:

activating iron powder, namely heating and activating the iron powder by using acid to obtain activated iron powder;

dissolving ferric chloride and ferrous chloride in water, adding ammonia water under the protection of nitrogen to form a precipitate, adjusting the pH value, heating for reaction, and separating a solid phase to obtain the composite magnetic particles;

liquid ingredients are prepared by adding 50-60 parts by weight of water into 1-3 parts by weight of magnetic particles, 1-3 parts by weight of oyster shell powder, 0.5-1.5 parts by weight of vitamin C, 0.5-1.0 parts by weight of tea polyphenol, 2-4 parts by weight of Arabic gum, 1-3 parts by weight of modified starch, 2-4 parts by weight of sodium chloride and 0.5-1.5 parts by weight of ethanol, and preparing a water mixed solution to obtain a liquid ingredient;

adding the liquid ingredient into paper pulp for papermaking, and feeding the paper pulp to a paper machine for papermaking;

the activated iron powder is sprayed on the surface of paper to prepare the deoxidizing preservative.

2. The method of claim 1, wherein the acid is hydrochloric acid or phosphoric acid.

3. The preparation method according to claim 2, wherein in the iron powder activation process, hydrochloric acid with a mass concentration of 5% to 25% is added, and iron powder with a mass concentration of 10% to 20% is added; the activation temperature of the iron powder is 100-150 ℃, and the activation time is 30-60 min.

4. The preparation method according to claim 1, wherein in the preparation process of the composite magnetic particles, ferric chloride and ferrous chloride are mixed according to a mass ratio of 1: 2-2: 1, and the total iron ion concentration is 0.1-0.3 mol/L.

5. The method according to claim 4, wherein the pH is maintained at l0 ± 0.1 by stirring, the reaction is carried out at 60-80 ℃ for 30-60 min, the solid phase is separated, washed with water to neutrality, washed with absolute ethanol, and dried at 70 ℃ under vacuum.

6. A method of manufacturing as claimed in claim 1, wherein the liquid furnish comprises 20-40% by mass of the pulp.

7. A method according to claim 6, characterized in that the liquid furnish is added to the pulp and sent to the paper machine for wire drainage, press dewatering and cylinder drying.

8. The preparation method of claim 1, wherein the activated iron powder is sprayed on the surface of paper, dried, calendered and cut to obtain the finished deoxidizing preservative.

9. A magnetic deoxidizing fresh-keeping agent prepared by the preparation method as described in any one of claims 1 to 8.