Microplastic pollution has become a global environmental problem. Textile microplastics are an important component of microplastic pollution, but little is known about their contamination in the industrial environment. The lack of standardized methods for detecting and quantifying textile microplastics is a major obstacle to determining the risks they pose to the natural environment. This study systematically examines the pretreatment options for the extraction of microplastics from printing and dyeing wastewater. The effectiveness of potassium hydroxide, nitric acid–hydrogen peroxide mixed solution, hydrogen peroxide, and Fenton’s reagent for the removal of organic matter from textile wastewater is compared. Three textile microplastics, polyethylene terephthalate, polyamide, and polyurethane, are studied. The effects of the digestion treatment on the physicochemical properties of textile microplastics are characterized. The separation efficiency of sodium chloride, zinc chloride, sodium bromide, sodium iodide, and sodium chloride-sodium iodide mixed solution on the textile microplastics is tested. The results showed that Fenton’s reagent achieved a 78% removal rate of organic matter from printing and dyeing wastewater. Meanwhile, it has less of an effect on the physicochemical properties of textile microplastics after digestion and is the best reagent for digestion. The zinc chloride solution achieved a 90% recovery for separating textile microplastics with good reproducibility. It does not affect the subsequent characterization analysis after separation and is the best solution for density separation.