Preparation method of paraffin inhibitor for oil wells

[0018] Example 1

[0019] First, weigh 1kg of papermaking black liquor and filter to obtain the filtrate. Add the filtrate to the beaker, and then add 60mL of 15% sulfuric acid solution to the beaker, and move the beaker into a digital speed constant temperature magnetic stirrer. Under the conditions of 110°C and 300r/min, the reaction was stirred at a constant temperature for 2 hours and then filtered to obtain the filter residue. Take 40 g of the filter residue and place it in a beaker containing 200 mL of a 5% sodium sulfite solution, and place the beaker in an oil bath. The temperature of the oil bath is controlled to 140℃, and the reaction is kept stirring for 3 hours. After the reaction is over, the materials in the beaker are placed in a rotary evaporator, and the material in the beaker is concentrated to dryness by rotary evaporation to obtain a dried product. Then take 20g of the dried product and add it to 100mL water Put the three-necked flask in a water bath, control the temperature of the water bath to 70℃, and pass nitrogen into the three-necked flask, control the inflow rate to 10mL/min, and then add 30mL to the three-necked flask. 25% hydrogen peroxide, controlled dropping rate of 1mL/min. After the addition of hydrogen peroxide is completed, after stirring and reacting for 40 minutes, add 10g acrylic acid to the three-necked flask, keep stirring and react for 2 hours, when the reaction is over, place the product in the rotary evaporator , Rotary steaming and concentrating for 35 minutes to obtain a concentrated solution. Weigh 800g potato starch and add it to a ball mill and ball mill for 30 minutes to obtain ball milled starch. Take 600g of ball milled starch and add it to a three-necked flask containing 1L of absolute ethanol. The flask is placed in a water bath, the temperature of the water bath is controlled to 50°C, and 8g of sodium periodate is added to the three-necked flask, and the reaction is kept for 3 hours. After the reaction is completed, it is filtered to obtain oxidized starch, and then 200g of oxidized starch is added to the container. In a beaker with 700 mL of water, add 10% sodium hydroxide solution to the beaker to adjust the pH of the material in the beaker to 9.2, then place the flask in a water bath, control the temperature of the water bath at 60 ℃, and add 100 mL dropwise to the beaker The mass fraction is 15% maleic anhydride ether solution, and the dropping rate is controlled to be 1mL/min. After the dripping is completed, the reaction is stirred for 2h. After the reaction is completed, filter to obtain a filter cake. Finally, take 10 parts by weight and concentrate Liquid, 20 parts of filter cake, 60 parts of isopropanol, 10 parts of propylene glycol butyl ether and 10 parts of ethylene glycol are added to the beaker, stirred and mixed for 15 minutes, and discharged to obtain the wax inhibitor for oil wells.

[0020] Example 2

[0021] First, weigh 1kg of papermaking black liquor and filter to obtain the filtrate, add the filtrate to the beaker, then add 70mL of 15% sulfuric acid solution to the beaker, and move the beaker into the digital display speed constant temperature magnetic stirrer, at the temperature Under the condition of 115°C and rotating speed of 350r/min, the reaction was stirred at constant temperature for 2 hours and then filtered to obtain the filter residue. Take 45g of the filter residue and place it in a beaker containing 250mL of 5% sodium sulfite solution and place the beaker in an oil bath. Control the temperature of the oil bath at 145℃, keep stirring and react for 3 hours. After the reaction is over, place the material in the beaker on a rotary evaporator, and evaporate and concentrate to dryness to obtain a dry product. Then take 25g of the dry product and add it to 150mL of water. Put the three-necked flask in a water bath, control the temperature of the water bath at 75℃, and pass nitrogen into the three-necked flask, control the inflow rate to 13mL/min, and then drop 35mL into the three-necked flask. 25% hydrogen peroxide, controlled dropping rate of 2mL/min. After the addition of hydrogen peroxide is completed, the reaction is stirred for 45min, then 13g acrylic acid is added to the three-necked flask, and the reaction is kept for 2h. After the reaction is over, place the product in the rotary evaporator , Rotary steaming and concentration for 40 minutes to obtain a concentrated solution. Weigh 850g of corn starch and add it to a ball mill and ball mill for 35 minutes to obtain ball milled starch. Take 650g of ball milled starch and add it to a three-necked flask containing 1L of absolute ethanol. The flask is placed in a water bath, and the temperature of the water bath is controlled to 55°C. Then 10g of sodium periodate is added to the three-necked flask, and the reaction is kept for 3h. After the reaction is completed, it is filtered to obtain oxidized starch, and then 250g of oxidized starch is added to the container. In a beaker with 750mL water, add 10% sodium hydroxide solution to the beaker to adjust the pH of the material in the beaker to 9.4, then place the flask in a water bath, control the temperature of the water bath to 65℃, and add 125mL dropwise to the beaker The mass fraction is 15% maleic anhydride ether solution, and the dropping rate is controlled to be 2mL/min. After the dripping is completed, the reaction is stirred for 2h. After the reaction is completed, filter to obtain a filter cake. Finally, take 13 parts by weight and concentrate Liquid, 25 parts of filter cake, 65 parts of isopropanol, 13 parts of propylene glycol butyl ether and 13 parts of ethylene glycol are added to the beaker, stirred and mixed for 18 minutes, and discharged to obtain the wax inhibitor for oil wells.

[0022] Example 3

[0023] First, weigh 2kg of papermaking black liquor and filter to obtain the filtrate, add the filtrate to the beaker, then add 80 mL of 15% sulfuric acid solution to the beaker, and move the beaker into the digital speed constant temperature magnetic stirrer. Under the conditions of 120°C and 400r/min, the reaction was stirred at a constant temperature for 3 hours and then filtered to obtain a filter residue. Take 50g of the filter residue and place it in a beaker containing 300 mL of a 5% sodium sulfite solution, and place the beaker in an oil bath. The temperature of the oil bath is controlled to 150℃, the temperature is kept and the reaction is stirred for 4 hours. After the reaction is over, the materials in the beaker are placed in a rotary evaporator, and the material in the beaker is concentrated to dryness by rotary evaporation to obtain a dried product. Then take 30g of the dried product and 0.5g of iron sulfate and add Into a three-necked flask containing 200mL of water, place the three-necked flask in a water bath, control the temperature of the water bath to 80°C, pour nitrogen into the three-necked flask, control the inflow rate to 15mL/min, and then drip into the three-necked flask Add 40mL of 25% hydrogen peroxide with a mass fraction of 25%, and control the drip rate to 3mL/min. After the addition of hydrogen peroxide is completed, stir and react for 50min, then add 15g of acrylic acid to the three-necked flask, keep it warm and stir for 3h. After the reaction is over, place the product In a rotary evaporator, the concentrated solution was obtained by rotary evaporation for 45 min. Weigh 900 g of wheat starch and add it to the ball mill and ball mill for 40 min to obtain the ball milled starch. Take 700 g of the ball milled starch and add it to a three-necked flask containing 2L of absolute ethanol. Put the three-necked flask in a water bath, control the temperature of the water bath to 60℃, then add 12g of sodium periodate to the three-necked flask, keep the temperature and stir for 4h, filter after the reaction is over, get oxidized starch, then take 300g of oxidized starch The starch was added to a beaker containing 800 mL of water, and a 10% sodium hydroxide solution was added to the beaker to adjust the pH of the material in the beaker to 9.5, then the flask was placed in a water bath, and the temperature of the water bath was controlled to 70°C. Add 150 mL of 15% maleic anhydride diethyl ether solution with a mass fraction of 15% to the beaker, and control the dripping rate to 3 mL/min. After the dripping is completed, stir and react for 3 hours. After the reaction, filter to obtain a filter cake, and finally calculate by weight , Take 15 parts of concentrated solution, 30 parts of filter cake, 3 parts of stearylamine polyoxyethylene ether, 70 parts of isopropanol, 15 parts of propylene glycol butyl ether and 15 parts of ethylene glycol into the beaker, stir and mix for 20 minutes, and then It can get wax inhibitor for oil well.