Phosphate leather fat liquoring agent and preparation method thereof

Abstract

The invention provides a phosphate leather fat liquoring agent and a preparation method thereof. A phosphorylated polyether modified aminosilicone leather fat liquoring agent is prepared by modifying aminosilicone with allyl polyether and P2O5 serving as raw materials. An active group phosphate radical in a molecular structure can react with an amino group in a leather fiber structure, and can be tightly combined with chromium in chrome tanned leather in the form of a coordination bond, so that a phosphorylation product can be stored in leather fiber for a long time, and leather is endowed with certain flame retardance and antistatic property. A certain quantity of hydrophilic oxyethyl groups are introduced onto the molecular structure, so that the properties of water solubility, acid resistance, electrolyte resistance and the like of aminosilicone are improved effectively, and the self-emulsifying property of aminosilicone is enhanced. Aminosilicone is a leather fat liquoring agent per se, and can be used for endowing leather with higher flexibility and fullness and enhancing the physical and mechanical properties such as tear resistance, thickening rate and the like of the leather; and the leather fat liquoring agent with the structure has higher development and application values.

Description

technical field

[0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a phosphate-based leather fatliquoring agent and a preparation method thereof. Background technique

[0002] The development and research of organic silicon products has been one of the research hotspots at home and abroad in the past ten years, and the leather industry is no exception, especially the famous foreign companies such as Dowcorning, Rohm&Hass, and BASF. ), Bayer, Clariant, Henkel, Kenneth Stahl and other companies have successfully developed a series of multifunctional silicone leather special products, including silicone water repellent, soft plus Fat agent, finishing agent.

[0003] Among many organosilicon compounds, amino silicone oil is a kind of "green" product that is non-toxic, non-environmentally polluting, and low in cost. However, limited by the hydrophobicity of amino silicone oil, emulsifiers must be used for emulsification before ...

Examples

Embodiment 1

[0032] The first step: allyl polyether modified amino silicone oil

[0033] Add 450 parts of allyl polyether and 1000 parts of amino silicone oil in parts by mass into a reactor equipped with a stirrer, condenser and thermometer, mix well, heat up, react at 60°C for 10 hours, cool to room temperature, and obtain activity Polyether modified amino silicone oil, the allyl polyether is APEG-500; the structural formula of the amino silicone oil is

[0034]

[0035] Indicates the siloxane chain, the amino value of amino silicone oil is 0.9mmol / g;

[0036] Step 2: Phosphorylation

[0037] Control the temperature at 30°C, slowly add 63.9 parts of P 2 o 5 , the feeding time is 1h, and then the temperature is slowly raised to 65°C, and the constant temperature is reacted for 5.5h to obtain phosphorylated polyether modified amino silicone oil;

[0038] Step Three: Neutralization

[0039] After the second step, neutralize the system with an alkaline aqueous solution until the pH...

Embodiment 2

[0041] The first step: allyl polyether modified amino silicone oil

[0042] Add 490 parts of allyl polyether and 1000 parts of amino silicone oil in parts by mass into a reactor equipped with a stirrer, condenser and thermometer, mix well, heat up, react at 60°C for 10 hours, cool to room temperature, and obtain activity Polyether modified amino silicone oil, the allyl polyether is APEG-700; the structural formula of the amino silicone oil is

[0043]

[0044] Indicates the siloxane chain, the amino value of amino silicone oil is 0.7mmol / g;

[0045] Step 2: Phosphorylation

[0046] Control the temperature at 20°C, slowly add 49.7 parts of P in batches to the reactor after the first step 2 o 5 , the feeding time is 1.5h, then the temperature is slowly raised to 60°C, and the constant temperature is reacted for 6h to obtain phosphorylated polyether modified amino silicone oil;

[0047] Step Three: Neutralization

[0048] After the second step, neutralize the system wit...

Embodiment 3

[0050] The first step: allyl polyether modified amino silicone oil

[0051] Add 500 parts of allyl polyether and 1000 parts of amino silicone oil in parts by mass into a reactor equipped with a stirrer, condenser and thermometer, mix well, heat up, react at 80°C for 6 hours, cool to room temperature, and obtain activity Polyether modified amino silicone oil, the allyl polyether is APEG-1000; the structural formula of the amino silicone oil is

[0052]

[0053] Indicates the siloxane chain, the amino value of amino silicone oil is 0.5mmol / g;

[0054] Step 2: Phosphorylation

[0055] Control the temperature at 25°C, slowly add 35.5 parts of P in batches to the reactor after the first step 2 o 5 , the feeding time is 2 hours, and then the temperature is slowly raised to 80 ° C, and the temperature is reacted for 3 hours to obtain phosphorylated polyether modified amino silicone oil;

[0056] Step Three: Neutralization

[0057]After the second step, neutralize the system...

technical field

[0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a phosphate-based leather fatliquoring agent and a preparation method thereof. Background technique

[0002] The development and research of organic silicon products has been one of the research hotspots at home and abroad in the past ten years, and the leather industry is no exception, especially the famous foreign companies such as Dowcorning, Rohm&Hass, and BASF. ), Bayer, Clariant, Henkel, Kenneth Stahl and other companies have successfully developed a series of multifunctional silicone leather special products, including silicone water repellent, soft plus Fat agent, finishing agent.

[0003] Among many organosilicon compounds, amino silicone oil is a kind of "green" product that is non-toxic, non-environmentally polluting, and low in cost. However, limited by the hydrophobicity of amino silicone oil, emulsifiers must be used for emulsification before ...

Examples

Embodiment 1

[0032] The first step: allyl polyether modified amino silicone oil

[0033] Add 450 parts of allyl polyether and 1000 parts of amino silicone oil in parts by mass into a reactor equipped with a stirrer, condenser and thermometer, mix well, heat up, react at 60°C for 10 hours, cool to room temperature, and obtain activity Polyether modified amino silicone oil, the allyl polyether is APEG-500; the structural formula of the amino silicone oil is

[0034]

[0035] Indicates the siloxane chain, the amino value of amino silicone oil is 0.9mmol / g;

[0036] Step 2: Phosphorylation

[0037] Control the temperature at 30°C, slowly add 63.9 parts of P 2 o 5 , the feeding time is 1h, and then the temperature is slowly raised to 65°C, and the constant temperature is reacted for 5.5h to obtain phosphorylated polyether modified amino silicone oil;

[0038] Step Three: Neutralization

[0039] After the second step, neutralize the system with an alkaline aqueous solution until the pH...

Embodiment 2

[0041] The first step: allyl polyether modified amino silicone oil

[0042] Add 490 parts of allyl polyether and 1000 parts of amino silicone oil in parts by mass into a reactor equipped with a stirrer, condenser and thermometer, mix well, heat up, react at 60°C for 10 hours, cool to room temperature, and obtain activity Polyether modified amino silicone oil, the allyl polyether is APEG-700; the structural formula of the amino silicone oil is

[0043]

[0044] Indicates the siloxane chain, the amino value of amino silicone oil is 0.7mmol / g;

[0045] Step 2: Phosphorylation

[0046] Control the temperature at 20°C, slowly add 49.7 parts of P in batches to the reactor after the first step 2 o 5 , the feeding time is 1.5h, then the temperature is slowly raised to 60°C, and the constant temperature is reacted for 6h to obtain phosphorylated polyether modified amino silicone oil;

[0047] Step Three: Neutralization

[0048] After the second step, neutralize the system wit...

Embodiment 3

[0050] The first step: allyl polyether modified amino silicone oil

[0051] Add 500 parts of allyl polyether and 1000 parts of amino silicone oil in parts by mass into a reactor equipped with a stirrer, condenser and thermometer, mix well, heat up, react at 80°C for 6 hours, cool to room temperature, and obtain activity Polyether modified amino silicone oil, the allyl polyether is APEG-1000; the structural formula of the amino silicone oil is

[0052]

[0053] Indicates the siloxane chain, the amino value of amino silicone oil is 0.5mmol / g;

[0054] Step 2: Phosphorylation

[0055] Control the temperature at 25°C, slowly add 35.5 parts of P in batches to the reactor after the first step 2 o 5 , the feeding time is 2 hours, and then the temperature is slowly raised to 80 ° C, and the temperature is reacted for 3 hours to obtain phosphorylated polyether modified amino silicone oil;

[0056] Step Three: Neutralization

[0057]After the second step, neutralize the system...

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